CN111905836B - Porous plastic chemical reagent carrier and preparation method and application thereof - Google Patents

Porous plastic chemical reagent carrier and preparation method and application thereof Download PDF

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Publication number
CN111905836B
CN111905836B CN202010819698.5A CN202010819698A CN111905836B CN 111905836 B CN111905836 B CN 111905836B CN 202010819698 A CN202010819698 A CN 202010819698A CN 111905836 B CN111905836 B CN 111905836B
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porous
carrier
reagent
porous plastic
chemical reagent
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CN111905836A (en
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胥波
齐义舟
李婷婷
齐培州
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Shanghai Group Wave Intelligent Instrument Technology Co ltd
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Shanghai Group Wave Intelligent Instrument Technology Co ltd
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    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/63—Pore volume
    • B01J35/633—Pore volume less than 0.5 ml/g
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    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
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    • C07C227/20—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters by hydrolysis of N-acylated amino-acids or derivatives thereof, e.g. hydrolysis of carbamates
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Abstract

The invention provides a porous plastic chemical reagent carrier, a preparation method and application thereof. The chemical reagent carrier prepared by the technical scheme changes the use form of the chemical reagent, so that solids, semisolids and viscous liquids which are difficult to operate and weigh accurately can be conveniently measured, the preparation process is simple and convenient, and no solvent which is not friendly to the environment is introduced in the preparation process, so that the chemical reagent carrier is easy to realize industrial production and has better environmental protection effect.

Description

Porous plastic chemical reagent carrier and preparation method and application thereof
Technical Field
The invention relates to the technical field of chemical reagent loading, in particular to a porous plastic chemical reagent carrier and a preparation method and application thereof.
Background
Chemical synthesis is increasingly used in various fields such as medicine, pesticide, fine chemical industry, materials, sensors, aerospace and the like. Despite significant advances, chemical synthesis is currently a fairly dangerous, labor-intensive industry. In particular, the potential safety hazards inherent in handling hazardous chemicals, which lead chemists in the field of chemical synthesis automation to the wisdom. While automation has completely changed many industrial and laboratory tasks, in practical applications, full automation of chemical synthesis has remained highly challenging, and in most schools and industrial laboratories, the vast majority of chemical experiments have still been accomplished manually. Many conventional chemical processing tasks remain difficult for automated machines to download or design a synthesis solution, and can be performed fully automatically in a local synthesizer, a dream of the synthesis chemist.
Because the chemical products involved in chemical synthesis are various, and the weighing of small or trace amounts of chemical reagents is time-consuming and labor-consuming, the automatic synthesis is realized, and thousands of reagents, especially the dosage of the reagents, need to be standardized first, so that the robot system for algorithm control is facilitated to use. Automated removal of low viscosity liquids is relatively easy, however, solid, semi-solid and viscous liquid reagents present significant challenges. In recent years, automated synthesis has been greatly progressed, but related researches at home and abroad have not been relatively general-purpose methods for processing thousands of chemicals with different forms, so that highly automated synthesis cannot be realized.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an ultrahigh molecular weight porous plastic chemical reagent carrier, and a preparation method and application thereof, and specifically adopts the following technical scheme:
the first aspect of the present invention provides a porous plastic chemical agent carrier which is a porous solid block structure;
Further, the porous plastic chemical reagent carrier is in a tablet-like cylindrical structure, a spherical structure or a cubic structure; further preferably, the porous plastic chemical reagent carrier with the tablet-like cylindrical structure has a pore volume of 0.3-0.6 ml/g, a total pore area of 20-25 m 2/g, an average pore diameter of 70-80 nm, a volume density of 0.5-1.0 g/ml at 0.5-1 psi and a porosity of 20-30%; preferably, the pore volume is 0.4298ml/g; the total pore area is 23.780m 2/g; the average pore diameter is 72.3nm; its bulk density at 0.5-1 psi 0.6069g/ml; the porosity is 26.0850%;
Further, the specification of the tablet-like cylindrical porous plastic chemical reagent carrier is as follows: the inner diameter is 5.1-9 mm and the height is 2.5-4 mm; further, the weight of the porous plastic chemical reagent carrier with the tablet-like cylindrical structure is 30 mg/tablet or 150 mg/tablet;
Further, the porous plastic is a material with high wear resistance and high chemical inertness, including but not limited to ultra-high molecular weight porous polyethylene, ultra-high molecular weight porous polypropylene, ultra-high molecular weight polytetrafluoroethylene or ultra-high molecular weight polytetrafluoroethylene;
Further, the chemical reagent is a solid reagent or a liquid reagent; still further, the solid reagent is a soluble solid or an insoluble solid; still further, the liquid reagents include, but are not limited to, viscous liquids;
The second aspect of the present invention provides a method for preparing the porous plastic chemical reagent carrier, comprising the following steps: adding the plastic powder into a cylindrical stainless steel grinding tool, heating to 140-155 ℃ under normal pressure, then rapidly cooling to room temperature, and removing the die to obtain the plastic powder;
Further, the diameter of the porous plastic powder is 10-100 mu m, and the molecular weight of the porous plastic powder is more than 100 ten thousand;
Further, the inner diameter of the cylindrical stainless steel grinding tool is 5.1-9 mm, and the height is 2.5-4 mm; specifically, the dimensions of the cylindrical stainless steel abrasive article: an inner diameter of 5.1mm and a height of 2.5mm, an inner diameter of 7.4mm and a height of 2.5mm or an inner diameter of 9mm and a height of 4mm;
in a third aspect the present invention provides the use of a porous plastic chemical agent carrier, characterised in that it is used to carry a chemical agent;
Further, the chemical reagent is a solid reagent or a liquid reagent; still further, the solid reagent is a soluble solid reagent or an insoluble solid reagent; still further, the liquid reagents include, but are not limited to, non-viscous liquid reagents or viscous liquid reagents.
A fourth aspect of the present invention provides a porous plastic chemical agent comprising the porous plastic chemical agent carrier described above and a chemical agent supported thereby, further wherein the amount of the substance of the chemical agent supported by the porous plastic chemical agent carrier is determined;
further, the porous plastic chemical reagent carrier carries 0.001 mu mol-10.0 mol of chemical reagent substances; further, the porous plastic chemical reagent carrier carries the chemical reagent with the amount of 0.01 mu mol-1.0 mol; further, the porous plastic chemical agent carrier carries a chemical agent in an amount of 0.001μmol、0.002μmol、0.005μmol、0.01μmol、0.02μmol、0.05μmol、0.1μmol、0.2μmol、0.5μmol、1μmol、2μmol、5μmol、10μmol、20μmol、50μmol、100μmol、200μmol、500μmol、1mmol、2mmol、5mmol、10mmol、20mmol、50mmol、100mmol、200mmol、500mmol or 1mol;
further, the porous plastic chemical reagent is a porous soluble solid reagent, a porous insoluble solid reagent or a porous liquid reagent; still further, the porous liquid reagents include, but are not limited to, porous non-viscous liquid reagents or porous viscous liquid reagents;
further, the preparation method of the porous soluble solid reagent comprises the following steps:
s1: dissolving soluble solid in low boiling point good solvent with the mass of 0.1-100% to prepare solution; preferably, the good solvent includes, but is not limited to, ethanol, chloroform or water;
S2: transferring the solution obtained in the step S1 to the porous plastic chemical reagent carrier by using a pipetting device, and obtaining a loaded solution porous carrier after the solution is completely adsorbed on the carrier; preferably, the pipetting device is a pipetting gun;
S3: vacuum drying the porous carrier of the load solution obtained in the step S2 at the pressure of 1mmHg and the temperature of 0-60 ℃ until the solvent is volatilized, thus obtaining the porous soluble solid reagent;
Further, in the porous dissolvable solid reagent, the amount of the substance of the porous plastic chemical reagent carrier loaded dissolvable solid reagent is 0.001 mu mol to 10.0mol; further, the porous plastic chemical reagent carrier carries soluble solid reagent substances in an amount of 0.01 mu mol to 1.0mol; still further, the porous plastic chemical agent carrier carries a soluble solid agent material in an amount of 0.001μmol、0.002μmol、0.005μmol、0.01μmol、0.02μmol、0.05μmol、0.1μmol、0.2μmol、0.5μmol、1μmol、2μmol、5μmol、10μmol、20μmol、50μmol、100μmol、200μmol、500μmol、1mmol、2mmol、5mmol、10mmol、20mmol、50mmol、100mmol、200mmol、500mmol or 1 mole;
Further, the preparation method of the porous insoluble solid reagent comprises the following steps:
s1: grinding the insoluble solid reagent into a powder below 5 microns;
S2: suspending the powder in an organic solvent with the mass of 8-50 times of that of the powder to obtain a suspension, adding the suspension into the porous plastic chemical reagent carrier while stirring at the speed of 300-600 r/min at the temperature of 0-30 ℃, and fully stirring for 1-24 h to enable the powder to be fully adsorbed to the carrier; preferably, the organic solvent includes, but is not limited to, ethanol, petroleum ether, toluene, tetrahydrofuran, or dichloromethane;
S3: continuously stirring the carrier obtained in the step S2 and loaded with the insoluble solid reagent in a clean and same organic solvent at the same speed and temperature for 10-24 hours to wash off unadsorbed powder on the surface of the carrier, namely the porous insoluble solid reagent; further, in the porous insoluble solid reagent, the amount of insoluble solid reagent substance carried by the porous plastic chemical reagent carrier is 0.001 mu mol to 10.0mol; further, the porous plastic chemical reagent carrier carries insoluble solid reagent substances in an amount of 0.01 mu mol to 1.0mol; still further, the porous plastic chemical agent carrier supports insoluble solid agent material in an amount of 0.001μmol、0.002μmol、0.005μmol、0.01μmol、0.02μmol、0.05μmol、0.1μmol、0.2μmol、0.5μmol、1μmol、2μmol、5μmol、10μmol、20μmol、50μmol、100μmol、200μmol、500μmol、1mmol、2mmol、5mmol、10mmol、20mmol、50mmol、100mmol、200mmol、500mmol or 1 mole.
Further, the loading method of the porous liquid reagent comprises the following steps:
S1: directly sucking a liquid reagent by a pipetting device or sucking liquid diluted to 5-100 times of the mass of the liquid reagent in a low-boiling point good solvent, dripping the liquid reagent on the porous plastic chemical reagent carrier, and obtaining a porous carrier for loading the liquid reagent after the carrier fully adsorbs the liquid reagent; preferably, the pipetting device is a pipetting gun;
S2: vacuum drying the porous carrier of the load solution obtained in the step S2 for 10 to 60 minutes under the conditions that the pressure is 1mmHg and the temperature is 0 to 60 ℃ to obtain the porous liquid reagent; further, in the porous liquid reagent, the amount of insoluble solid reagent substances loaded on the porous plastic chemical reagent carrier is 0.001 mu mol-10.0 mol; further, the porous plastic chemical reagent carrier carries insoluble solid reagent substances in an amount of 0.01 mu mol to 1.0mol; still further, the determined amount of liquid reagent material is 0.01μmol、0.02μmol、0.05μmol、0.1μmol、0.2μmol、0.5μmol、1μmol、2μmol、5μmol、10μmol、20μmol、50μmol、100μmol、200μmol、500μmol、1mmol、2mmol、5mmol、10mmol、20mmol、50mmol、100mmol、200mmol、500mmol or 1 mole.
Advantageous effects
The technical scheme adopted by the invention has the following technical effects:
The strength and the load capacity of the chemical reagent carrier are improved: porous plastics, in particular ultra high molecular weight Polyethylene (HIGH DENSITY Polyethylene, abbreviated HDPE), are white powder or granular products. No toxicity and smell, the crystallinity is 80-90%, the softening point is 125-l 35 ℃, and the use temperature can reach 110 ℃; hardness, tensile strength and creep are all superior to low density polyethylene; the wear resistance, the electrical insulation property, the toughness and the cold resistance are good; has good chemical stability, is insoluble in any organic solvent at room temperature, and has low acid, alkali and various salts corrosion resistance. Therefore, the carrier used for preparing the porous polymer chemical reagent has the following excellent technical effects:
the use form of the chemical reagent is changed, for example, liquid or soluble solid reagent is changed into solid reagent, and the reagent which is difficult to treat such as viscous liquid is changed into solid reagent, so that the reagent is convenient to use and convenient to quantify, and meanwhile, the reagent is also easy to separate from other chemical reagents; the transportation is convenient, and the contact between scientific researchers and toxic reagents can be reduced; the mechanical strength of the chemical reagent is obviously improved; the load capacity of the unit mass is large, which is favorable for the chemical reaction, and can be widely applied to various chemical reactions.
The preparation method of the porous plastic carrier is simpler and more convenient: the porous plastic carrier can be obtained through the operations of heating, sintering, cooling and the like under normal pressure; the method for loading the chemical reagent is simple and convenient: the chemical reagent can be loaded by dripping absorption or stirring at normal temperature and normal pressure; in addition, no solvent which is not friendly to the environment is introduced in the preparation process, so that the environment-friendly effect is better.
Drawings
FIG. 1 is a photograph of a blank chemical reagent carrier in real time and a scanning SEM image
FIG. 2 topographical features of Pd/C@tab prepared in example 2
FIG. 3 kinetic graph comparison of reagent tablets and reagent powders
Detailed Description
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
EXAMPLE 1 preparation of ultra high molecular weight porous polyethylene chemical reagent Carrier
The method comprises the following steps: adding ultra-high molecular weight polyethylene powder with the diameter of 50 mu m and the molecular weight of more than 100 ten thousand into a cylindrical stainless steel grinding tool with the inner diameter of 5.1, 7.4 or 9mm and the height of 2.5 or 4mm, heating to 150 ℃ under normal pressure, then rapidly cooling to room temperature, and removing the die to obtain the product. The prepared ultra-high molecular weight porous polyethylene chemical reagent carrier has high hardness, hardly breaks in the stirring process, but can be cut by a sharp knife to prepare various shapes, and the physical photos of the catalyst carrier with two diameters prepared in the embodiment 1 of the invention are shown in figure 1 a; the obtained carrier was placed under a scanning electron microscope and the SEM image obtained was as shown in fig. 1 b.
EXAMPLE 2 quantitative preparation of porous polyethylene chemical reagent tablets
(1) Preparation of Pd (OAc) 2 reagent tablets: 6.74mg of Pd (OAc) 2 was weighed and dissolved in 600. Mu.L of chloroform and mixed uniformly to prepare Pd (OAc) 2 solution, 20. Mu.L of the solution was precisely sucked by a pipette and dropped onto 30 blank slides (size: diameter: 5.1 mm. Times.2.5 mm,30 mg/tablet) respectively, and after sufficient absorption, the content of Pd (OAc) 2 in the prepared reagent tablets was 1. Mu. Mol/tablet.
(2) Preparation of XPhos reagent tablets: weighing 14.28mg XPhos, dissolving in 600 mu L chloroform, mixing to obtain XPhos solution, precisely sucking 20 mu L of the solution with a pipette, respectively dripping onto 30 blank load slides (size: diameter: 5.1 mm. Times.2.5 mm,30 mg/tablet), fully absorbing, and vacuum drying to obtain a reagent tablet with XPhos content of 1 mu mol/tablet.
(3) Preparation of K 3PO4 reagent tablets: 636.80mg of K 3PO4 is weighed and dissolved in 1.8mL of water, the solution is uniformly mixed, 60 mu L of solution is respectively dripped on 30 blank load slides (size: 9.0mm x 4mm,150 mg/tablet) by a pipette gun, 20 mu L of ethanol is dripped to drive the water solution to be absorbed by the load slide, and the content of the prepared reagent tablet K 3PO4 is 0.1 mmol/tablet after vacuum drying.
(4) Preparation of various ligand reagent tablets. The preparation method is the same as that of K 3PO4. PPh 3, SPhos, xtantPhos, DPEPhos, dppf were prepared as respective chloroform solutions and prepared into reagent tablets (size: diameter 5.1 mm. Times.2.5 mm,30 mg/tablet) each having a ligand content of 1. Mu. Mol/tablet.
(5) Preparation of sodium tert-butoxide reagent tablets: the preparation method is the same as that of K 3PO4. The sodium tert-butoxide was weighed and prepared into a THF solution to prepare reagent tablets of two specifications of 0.05 mmol/tablet (size: diameter 5.1 mm. Times. Height 2.5mm,30 mg/tablet) and 0.2 mmol/tablet (size: diameter 5.1 mm. Times. Height 2.5mm,30 mg/tablet), respectively. The preparation method is the same as that of K 3PO4.
(6) Preparation of Pd/C reagent tablets: 600.0mg of micro Pd/C powder (commercial available, pd content is 10 wt/wt%) is ground into powder with a particle size less than or equal to 5 μm, then the powder is suspended in 150ml of ethanol, then 100 pieces (size: diameter 5.1 mm. Times.2.5 mm,30 mg/piece) of porous plastic chemical reagent carrier are added with stirring, the stirring speed is 500r/min, the stirring temperature is room temperature, and the stirring time is 24h; fully stirring to enable the reagent to be fully loaded on the carrier until the suspension becomes clear, then taking out the loaded reagent, continuously stirring in clean 100mL of ethanol for 12 hours at the same speed and temperature to wash off the redundant reagent on the surface of the catalyst carrier, and obtaining Pd/C@tab, wherein the maximum load of the carrier on the micron Pd/C is 2 mu mol/tablet; the photograph of the quantitative Pd/C@tab obtained is shown in FIG. 2.
EXAMPLE 3 Suzuki reaction and kinetic study thereof
Into a reaction tube were placed a powder reagent substrate 4-bromoanisole (0.1 mmol,18.7 mg), 1-naphthalene boric acid (0.1 mmol,17.2 mg), and palladium acetate reagent tablets (1 tablet), XPhos reagent tablets (2 tablets), K 3PO4 reagent tablets (2 tablets) prepared in example 2, ethanol aqueous solution (ethanol: water volume ratio 9:1) 1.5mL; a separate reaction tube was charged with 4-bromoanisole (0.1 mmol,18.7 mg), 1-naphthalene boronic acid (0.1 mmol,17.2 mg), palladium acetate (1. Mu. Mol,0.22 mg), XPhos (2. Mu. Mol,0.95 mg), K 3PO4 (0.2 mmol,42.45 mg) and aqueous ethanol (ethanol: water volume ratio 9:1) in 1.5mL. The two reaction tubes are simultaneously stirred at 60 ℃, when the reaction is respectively carried out for 15min, 30min, 1h, 2h and 4h, reaction solution is respectively taken and the conversion rate of the reaction is detected by GC-MS to obtain a reaction kinetic diagram (shown in figure 3), and as can be seen from figure 3, the palladium acetate reagent sheet, the XPhos reagent sheet, the K 3PO4 reagent sheet, the palladium acetate, the XPhos and the K 3PO4 powder are respectively adopted for reaction, and the conversion rates of the two reactions are extremely similar at the same moment, so that the introduction of the reagent sheet does not influence the release of the reagent and the reaction rate.
Example 4 Loading sheet for other chemical Agents
Using very similar methods, reagent tablets as shown in table 1 were prepared:
example 5: olefin metathesis reactions
To the reaction flask was added a solution of 1-octene in dichloromethane (abbreviated as DCM) (2 mL,0.1 mol/L), ethyl acrylate (173.9. Mu.L, 1.6 mmol) and 2 Grubbs catalyst support plates (0.001 mmol/plate). The mixture was stirred at room temperature under argon for 5 hours. After removal of the tablet, the reaction mixture was evaporated on a high vacuum pump and the crude product was purified by flash chromatography on a silica gel column (eluent: hexane/ethyl acetate v/v=20:1) to give compound 2-enenonethyl ester (35.4 mg, 96% yield). Nuclear magnetic spectrum identification shows that the compound 2-enanonylethyl ester 1H-NMR(400MHz,CDCl3)δ：7.04-6.91(m,1H),5.81(d,J＝15.7Hz,1H),4.19(q,J＝6.8Hz,2H),2.19(d,J＝6.5Hz,2H),1.50-1.20(m,11H),0.89(t,J＝6.8Hz,3H).
Example 6: photo-delay reaction
To the reaction flask were added a THF solution of p-nitrobenzoic acid, phenethyl alcohol (24.0. Mu.L, 0.2 mmol), 2 PPh 3 -carrying sheets (0.2 mmol/sheet) and 2 diethyl azodicarboxylate-carrying sheets (DEAD-carrying sheets, 0.2 mmol/sheet); after stirring the mixture at room temperature overnight and taking out the tablet, the reaction mixture was evaporated on a high vacuum pump and the crude product was purified by flash chromatography on a silica gel column (eluent: hexane/ethyl acetate v/v=10:1) to give the compound phenethyl p-nitrobenzoate (44.1 mg, 81% yield). Nuclear magnetic spectrum identification shows that the compound p-nitrophenyl ethyl benzoate 1H NMR(400MHz,CDCl3)：δ8.28(d,J＝8.7Hz,2H),8.17(d,J＝8.7Hz,2H),7.40-7.19(m,5H),4.59(t,J＝6.9Hz,2H),3.11(t,J＝6.9Hz,2H).
Example 7: trifluoromethyl reaction
To the reaction flask were added methyl benzoate (25.0 μl,0.2 mmol), trifluoromethyl trimethylsilane (abbreviated as TMS-CF 3, 32.5 μl,0.23 mmol) and 1 cesium fluoride load slide (CsF-load slide, 0.002 mmol/slide), and the mixture was stirred at room temperature and monitored by 19 F NMR; after completion, the resultant product was extracted with diethyl ether (10 mL), and diethyl ether was removed to give the product trifluoroacetophenone (44.1 mg, yield 81%), which was confirmed by nuclear magnetic resonance spectroscopy ,1H NMR(400MHz,CDCl3)δ8.08(d,J＝8.4Hz,2H),7.72(t,J＝6.9Hz,1H),7.56(t,J＝7.9Hz,2H);19F NMR(400MHz,CDCl3)δ71.42(s).
Example 8: cyclization reaction
To the reaction flask were added ethanol-free chloroform (0.5 mol/L,1 mL), styrene (23.0. Mu.L, 0.2 mmol), and nitromethylbenzene, 1 piece of 1, 4-diazabicyclo [2.2.2] octane (DABCO-loading sheet, 0.1 mmol/piece), and the mixture was stirred at 60℃for 40 hours. The solvent was then removed, the residue was dissolved in diethyl ether (10 mL) and washed with water (3×10 mL), naOH (1 m,3×10 mL) and brine (3×10 mL), and the organic layer was dried over Na 2SO3 and concentrated; the crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v=10:1) to give the product 3, 5-diphenyl-4, 5-dihydroisoxazole-in (35.7 mg, 80% yield). The product is identified by nuclear magnetic resonance spectrum ,1H NMR(400MHz,CDCl3)δ7.73-7.66(m,2H),7.45-7.29(m,8H),5.74(dd,J＝11.0,8.2Hz,1H),3.78(dd,J＝16.6,11.0Hz,1H),3.35(dd,J＝16.6,8.2Hz,1H).
Example 9: substitution reaction
To the reaction flask were added acetonitrile solution (0.1 mol/L,2 mL), ethylene glycol (278.8. Mu.L, 5 mmol) and 4 pieces of silver p-toluenesulfonate (AgOTs-loading sheet, 0.1 mmol/piece of 1 '-bromo-2', 3',6',2, 3,4, 6-heptyl-o-acetyl- α -d-lactose, the mixture was stirred at room temperature for 3 hours, after filtering the solid, the solvent was evaporated and the crude product was dissolved in ethyl acetate (ethyl acetate, 5 mL), the solution was washed with water (3X 5 mL), and the aqueous layer was back-extracted with ethyl acetate (10 mL), the combined organic layers were dried over anhydrous sodium sulfate and concentrated, and the crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v=1:1) to give disaccharide (86.5 mg, 65% yield) as shown in formula 24. The product is identified by nuclear magnetic resonance spectroscopy, and the product is identified by nuclear magnetic resonance spectroscopy ,1H NMR(400MHz,CDCl3)δ5.35(d,J＝3.4Hz,1H),5.21(t,J＝9.3Hz,1H),5.12(dd,J＝10.4,7.8Hz,1H),5.00-4.87(m,2H),4.58-4.45(m,3H),4.09(ddd,J＝23.6,11.7,5.2Hz,4H),3.92-3.82(m,2H),3.82-3.63(m,5H),2.16(s,3H),2.13(s,3H),2.08-2.03(m,12H),1.97(s,3H).
Example 10: hydrogenation reaction
To a reaction flask, an ethanol solution (0.1 mol/L,2 mL) of N-benzyloxycarbonyl-L-phenylalanine (N-Cbz-L-phenylalanine) was added 6 Pd/C-loading tabs (0.001 mmol/tablet). The mixture was stirred at room temperature under an atmosphere of H2 (balloon) for 4 hours. After removal of the tablets, the combined solution was concentrated in vacuo to give the pure product, which was phenylalanine (29.5 mg, 89%) without further purification. The product is identified by nuclear magnetic resonance spectrum ,1H NMR(400MHz,D2O)δ7.44-7.26(m,5H),3.96(dd,J＝8.0,5.2Hz,1H),3.26(dd,J＝14.5,5.2Hz,1H),3.10(dd,J＝14.5,8.0Hz,1H).
EXAMPLE 5 reductive amination
To the reaction flask, tetrahydro-4H-pyran-4-one (18.5. Mu.L, 0.2 mmol), benzylamine (24.0. Mu.L, 0.22 mmol) and titanium isopropoxide (94.7. Mu.L, 0.32 mmol) were added and stirred. At room temperature for 3 hours. Thereafter, 3 NaBH 4 -supported tablets (0.1 mmol/tablet) were added. The mixture was stirred for 24 hours. After removal of the tablets, sodium hydroxide solution was added and the mixture was extracted with DCM (3×5 mL) and then washed with brine (5 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v=5:1) to give N-benzyl-tetrahydropyran-4-amine (35.8 mg, 93% yield). The product is identified by nuclear magnetic resonance spectrum ,1H NMR(CDCl3)δ7.22-7.36(m,5H),3.98(d,J＝11.7Hz,2H),3.83(s,2H),3.38(t,J＝11.6Hz,2H),2.67-2.77(m,1H)),1.86(d,J＝11.5Hz,2H),1.38-1.50(m,2H).
EXAMPLE 5 condensation reaction
To the reaction flask were added propiolic acid (13.5 μl,0.22 mmol), N-methylaniline (21.7 μl,0.2 mmol), 1 dicyclohexylcarbodiimide slide (DCC-slide, 0.15 mmol/tablet) and 2 pieces of 4-dimethylaminopyridine (DMAP-slide, 0.01 mmol/tablet) and DCM (2 mL). The mixture was stirred at room temperature overnight. After filtering the solid, the reaction mixture was evaporated on a high vacuum pump and the crude product was purified by flash chromatography on a silica gel column (eluent: hexane/ethyl acetate v/v=10:1) to give the product N-phenyl-N-methyl-propynylamine (27.8 mg, 87% yield). The product is identified by nuclear magnetic resonance spectrum ,1H NMR(400MHz,CDCl3)δ7.45-7.36(m,3H),7.29(dd,J＝7.7,1.5Hz,2H),3.34(s,3H),2.81(s,1H).
EXAMPLE 5 reduction reaction
To the reaction flask were added estrone in ethanol (0.1 mol/L,2 mL) and 2 NaBH 4 -loaded tablets (0.1 mmol/tablet). The mixture was stirred at room temperature for 2h. After removal of the tablets, water (10 mL) was added and the aqueous phase extracted with ethyl acetate (3 x 5 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v=2:1) to give sterol (49.5 mg, yield 91%). The product is identified by nuclear magnetic resonance spectrum ,1H NMR(400MHz,Methanol-d4)δ7.07(d,J＝8.4Hz,1H),6.56-6.43(m,2H),3.65(t,J＝8.6Hz,1H),2.76(d,J＝5.0Hz,2H),2.29(d,J＝15.8Hz,1H),2.07-1.81(m,3H),1.69(dd,J＝7.0,2.6Hz,1H),1.57-1.13(m,8H),0.77(s,3H).
EXAMPLE 5 allylation reaction
To the reaction flask were added a DMF solution of 4-methoxyphenol 36 (0.1 mol/L,2 mL), allyl bromide (20.8. Mu.L, 0.24 mmol) and 2K 2CO3 -carrying tablets (0.2 mmol/tablet). The mixture was stirred at 70℃for 16 hours. After removal of the tablets, the reaction was quenched with water (5 mL) and extracted with diethyl ether (2X 5 mL). The combined organic extracts were washed with brine (2×5 mL), dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate v/v=10:1) to give p-methoxyphenol allyl ether (32.1 mg, yield 98%). The product is identified by nuclear magnetic resonance spectrum ,1H NMR(400MHz,CDCl3)δ6.88-6.79(m,4H),6.05(tdd,J＝17.3,10.6,5.3Hz,1H),5.40(ddd,J＝17.3,3.0Hz,1.3Hz,1H),5.27(ddd,J＝10.6,3.0Hz,1.3Hz,1H),4.48(td,J＝1.3and 5.3Hz,2H),3.76(s,3H).
EXAMPLE 5 condensation reaction
The reaction flask was charged with bicyclo [2.2.1] hept-5-ene-2-carbaldehyde (23.7. Mu.L, 0.2 mol), malononitrile (12.6. Mu.L, 0.2 mmol), 1 pyridine slide (Py slide, 0.04 mmol/piece), glacial acetic acid (2 mL). The mixture was stirred at room temperature overnight. After removal of the tablets, the reaction was quenched with water (5 mL) and extracted with ethyl acetate (3×5 mL). The combined organic extracts were washed with water (10 mL), dried over anhydrous sodium sulfate and concentrated. The crude product was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate v/v=10:1) to give the product bicyclo [2.2.1] -5-hepten-2-methylenemalonaldehyde (32.5 mg, 88%). The product is identified by nuclear magnetic resonance spectrum ,1H NMR(400MHz,400MHz,CDCl3)δ6.85(d,J＝11.0Hz,1H),6.36(dd,J＝5.7,3.1Hz,1H),6.00(dd,J＝5.7,2.8Hz,1H),3.37-3.28(m,1H),3.07(d,J＝15.7Hz,2H),2.19(ddd,J＝12.4,9.1,3.5Hz,1H),1.60(d,J＝8.1Hz,1H),1.42(d,J＝8.7Hz,1H),0.96(ddd,J＝12.2,3.8,2.6Hz,1H).
While the invention has been described with reference to the preferred embodiments, it is not limited thereto, and various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (3)

1. The porous plastic chemical reagent carrier is characterized in that the porous plastic chemical reagent carrier is of a tablet-like cylindrical structure, the pore volume of the porous plastic chemical reagent carrier is 0.3-0.6 ml/g, the total pore area of the porous plastic chemical reagent carrier is 20-25 m 2/g, the average pore diameter of the porous plastic chemical reagent carrier is 70-80 nm, the volume density of the porous plastic chemical reagent carrier at 0.5-1 psi is 0.5-1.0 g/ml, and the porosity of the porous plastic chemical reagent carrier is 20-30%; and the specification of the tablet-like cylindrical structure porous plastic chemical reagent carrier is as follows: the inner diameter is 5.1-9 mm and the height is 2.5-4 mm; and the weight of the porous plastic chemical reagent carrier with the tablet-like cylindrical structure is 30 mg/tablet or 150 mg/tablet; the porous plastic is ultrahigh molecular weight porous polyethylene;
The preparation method of the porous plastic chemical reagent carrier comprises the following steps: adding porous plastic powder into a cylindrical stainless steel grinding tool, heating to 140-155 ℃ under normal pressure, then rapidly cooling to room temperature, and removing the die to obtain the stainless steel grinding tool, wherein the diameter of the porous plastic powder is 10-100 mu m, the molecular weight of the porous plastic powder is more than 100 ten thousand, and the inner diameter of the cylindrical stainless steel grinding tool is 5.1-9 mm and the height of the cylindrical stainless steel grinding tool is 2.5-4 mm.
2. A porous plastic chemical reagent, characterized in that the porous plastic chemical reagent carrier of claim 1 and the chemical reagent carried thereby; the porous plastic chemical reagent carrier carries 0.01 mu mol-1.0 mol/piece of chemical reagent; the porous plastic chemical reagent is a porous soluble solid reagent, a porous insoluble solid reagent or a porous liquid reagent;
wherein,
The preparation method of the porous soluble solid reagent comprises the following steps: s1: dissolving the soluble solid in 0.1-100% of ethanol, chloroform or water to prepare a solution; s2: transferring the solution obtained in the step S1 to the porous plastic chemical reagent carrier by using a pipetting device, and obtaining a loaded solution porous carrier after the solution is completely adsorbed on the carrier; s3: vacuum drying the porous carrier of the load solution obtained in the step S2 at the pressure of 1mmHg and the temperature of 0-60 ℃ until the solvent is volatilized, thus obtaining the porous soluble solid reagent;
The preparation method of the porous insoluble solid reagent comprises the following steps: s1: grinding the insoluble solid reagent into a powder below 5 microns; s2: suspending the powder in an organic solvent of ethanol, petroleum ether, toluene, tetrahydrofuran or dichloromethane which is 8-50 times of the powder in mass to obtain a suspension, adding the suspension into the porous plastic chemical reagent carrier at the speed of 300-600 r/min under the condition of stirring at the temperature of 0-30 ℃, and fully stirring for 1-24 h to enable the powder to be fully adsorbed to the carrier; s3: continuously stirring the carrier obtained in the step S2 and loaded with the insoluble solid reagent in a clean and same organic solvent at the same speed and temperature for 10-24 hours to wash off unadsorbed powder on the surface of the carrier, namely the porous insoluble solid reagent;
The preparation method of the porous liquid reagent comprises the following steps: s1: directly sucking a liquid reagent by a pipetting device or sucking liquid diluted to 5-100 times of the mass of the liquid reagent in a low-boiling point good solvent, dripping the liquid reagent on the porous plastic chemical reagent carrier, and obtaining a porous carrier for loading the liquid reagent after the carrier fully adsorbs the liquid reagent; s2: and (3) vacuum drying the loaded solution porous carrier obtained in the step S2 for 10-60 min under the conditions that the pressure is 1mmHg and the temperature is 0-60 ℃ to obtain the porous liquid reagent.
3. The porous plastic chemistry of claim 2, wherein the pipetting device is a pipette gun.
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DE1694152C3 (en) * 1967-05-12 1979-09-13 Bayer Ag, 5090 Leverkusen Process for the production of microporous sheet-like structures
CA1308356C (en) * 1986-03-31 1992-10-06 Patrick P. Deluca Porous microspheres for drug delivery and method for making same
JP3559109B2 (en) * 1995-07-18 2004-08-25 三菱樹脂株式会社 Method for producing porous body made of ultra-high molecular weight polyethylene
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US5118648A (en) * 1988-10-05 1992-06-02 Mobil Oil Corporation Particulate polymer-supported olefin polymerization catalyst
JPH093236A (en) * 1995-06-15 1997-01-07 Mitsui Petrochem Ind Ltd Ultra high molecular weight polyethylene porous body
CN107649181A (en) * 2017-08-30 2018-02-02 北京工业大学 The preparation and application of a kind of heterogeneous fenton catalyst of support type based on teflon-coated

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