IES87061B2 - Peroxide second tertbutyl [Di-tert-butyl peroxide] organic intermediates synthesis method - Google Patents
Peroxide second tertbutyl [Di-tert-butyl peroxide] organic intermediates synthesis method Download PDFInfo
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- IES87061B2 IES87061B2 IES20180255A IES87061B2 IE S87061 B2 IES87061 B2 IE S87061B2 IE S20180255 A IES20180255 A IE S20180255A IE S87061 B2 IES87061 B2 IE S87061B2
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- 150000002978 peroxides Chemical class 0.000 title claims abstract description 21
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 title claims abstract description 18
- 239000000543 intermediate Substances 0.000 title claims abstract description 16
- 238000001308 synthesis method Methods 0.000 title claims abstract description 16
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 title abstract 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 16
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims abstract description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 7
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims abstract description 6
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 229940095564 anhydrous calcium sulfate Drugs 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 201000004569 Blindness Diseases 0.000 description 1
- 208000020564 Eye injury Diseases 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses peroxide second tert butyl [Di-tert-butyl peroxide] organic intermediates synthesis method, comprises the following steps:2-methyl-2-propylamine, potassium sulfate solution were added to the reaction vessel, controlled the mixing speed at 110-130rpm, controlled the reaction temperature of the solution to 5-10°C, added isopropyl alcohol aluminum, added the second glycol two ethyl ether solution in batches in 30-50min, continued to react for 90-120min;then added nickel fluoride power, controlled the mixing speed at 220-250rpm to react for 2-4h, let stand for 30-50min, layered, washed with sodium chloride solution for30-40min, washed with 1-pentanol solution for 20-40min, recrystallized in 2-hexone solution, dehydrated with dehydration, got the finished product peroxide second tert butyl.
Description
Peroxide second tertbutyl urgame intermediates synthesis method
FIELD OF THE INVENTION
The present invention relates to a method for preparing a pharmaceutical 5 intermediate which belongs to the field of organic synthesis, more particularly, relates to peroxide second tertbutyl organic intermediates synthesis method.
GENERAL BACKGROUND
Peroxide second tert butylas cross-linking agentcan be used in silicone rubber, synthetic rubber and natural rubber, polyethylene, EVA and EPT. As polymerization 10 initiator, it can be used in polystyrene and polyethylene. Most of the existing synthesis method adopt tertbutyl as raw material, and under the action of sulfuric acid, the hydrogen peroxide reaction with hydrogen peroxide is produced, and the reaction of tertbutyl hydrogen peroxide can be made with tertbutyl alcohol. But it need to use the synthetic method of sulfuric acid, hydrogen peroxide as raw materials, reaction raw 15 sulfuric acid corrosion resistance is stronger, the production equipment corrosion resistant ability of the demand is higher, health hazards for the operation personnel also is large, it is not conducive to safety production. The hydrogen peroxide of reactive materials is an explosive and powerful oxidizer, In the sealed container of suitable temperature, the gas phase explosion can be generated. Hydrogen peroxide 20 has a strong corrosive effect. Inhalation of steam or fog is strongly irritating to the airway. Direct contact with liquid can cause irreversible damage and even blindness. These increase the risk factor for the synthesis process and are not conducive to safe production. The above analysis shows that there are many deficiencies in this synthesis method, so it is necessary to put forward a new synthetic method.
SUMMARY
Based on the technical problems of the background technology, the purpose of the present invention is to provide peroxide second tert butyl organic intermediates synthesis method, comprises the following steps:
A: 2-methyl-2-propylamine, potassium sulfate solution were added to the reaction 30 vessel, controlled the mixing speed at 110-130 rpm, controlled the reaction temperature of the solution to 5-10’C, added isopropyl alcohol aluminum, added ths second glycol two ethyl ether solution in batches in 30-50min, continued to react for 90-120min;
B:then added nickel fluoride power, controlled the mixing speed at220-250rpm to react for 2-4h, let stand for 30-50min, layered, washed with sodium chloride solution for30-40min, washed with 1-pentanol solution for 20-40min, recrystallized in 2-hexone solution, dehydrated with dehydration, got the finished product peroxide second tert butyl.
Preferably, the potassium sulfate solution has a mass fraction of 10-16%.
Preferably, the mass fraction of second glycol two ethyl ether solution is 20-25%.
Preferably, the sodium chloride solution has a mass fraction of 15-21%.
Preferably, the 1-pentanol solution has a mass fraction of 40-46%.
Preferably, the mass fraction of 2-hexone solution is 60-65%,
Throughout the reaction process can be the following reaction formula:
Compared with the synthetic method disclosed in the background art, the invention provides peroxide second tert butyl organic intermediates synthesis method, it do not need to use sulfuric acid, hydrogen peroxide as raw materials, to avoid the reaction of raw materials for sulfuric acid corrosion damage to the equipment as well as the harm to the health of the operation personnel. It also avoids the risk of hydrogen gas explosion from strong oxidant hydrogen peroxide and hydrogen peroxide strong corrosive production operators respiratory and eye injury risk. It can reduce a lot of the reaction of the intermediate links, shorten the reaction time, and also improve reaction yield, at the same time, the present invention provides a new synthetic route which has laid a good foundation for further enhancing the yield of the reaction.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENT’S
The following examples with reference to specific embodiment of the present invention are further illustrated:
Embodiment 1
Peroxide second tert butyl organic intermediates synthesis method, comprises the following steps:
A:2mol2-methyl-2-propylamine, and 900ml potassium sulfate solution with a mass fraction of 10%were added to the reaction vessel, controlled the mixing speed at
HOrpm, controlled the reaction temperature of the solution to 5°C, added 4mol isopropyl alcohol aluminum, added 4mol the second glycol two ethyl ether solution wi th a mass fraction of 20% in two batches in 30mm, continued to react for 90mm;
B:then added 2mol nickel fluoride power, controlled the mixing speed at220rpm to react for 2h, let stand for 30min, layered, washed with sodium chloride solution with a mass fraction of 15% for30min, washed with 1-pentanol solution with a mass fraction of 40% for 20min, recrystallized in 2-hexone solution with a mass fraction of 60%, dehydrated with anhydrous calcium sulfate dehydration, got the finished product peroxide second tert buty!285.284g-. yield of 97.7%.
Embodiment 2
Peroxide second tert butyl organic intermediates synthesis method, comprises the following steps:
A:2mol 2-methyl-2-propylamine, and 900ml potassium sulfate solution with a mass fraction of 13%were added to the reaction vessel, controlled the mixing speed at 20 120rpm, controlled the reaction temperature of the solution to 7°C, added 5mol isopropyl alcohol aluminum, added. 5mol the second glycol two ethyl ether solution with a mass fraction of 23% in three batches in 40mm, continued to react for 1 OOmin;
B:then added 3mol nickel fluoride power, controlled the mixing speed at230rpm to react for 3h, let stand for 40min, layered, washed with sodium chloride solution 25 with a mass fraction of 18% for35min, washed with 1-pentanol solution with a mass fraction of 43% for 30min, recrystallized in 2-hexone solution with a mass fraction of 63%, dehydrated with anhydrous calcium sulfate dehydration, got the finished product peroxide second tert buty!285.868g, yield of 97.9%.
Embodiment 3
-’9 Peroxide second tert butyl organic intermediates synthesis method, comprises the following steps:
A:2mol 2-methyl-2-propylamine, and 900ml potassium sulfate solution with a mass fraction of 16%were added to the reaction vessel, controlled the mixing speed at 130rpm, controlled the reaction temperature of the solution to 10’C, added 6mol 5 isopropyl alcohol aluminum, added 6moi the second glycol two ethyl ether solution with a mass fraction of 25% in four batches in 50min, continued to react for 120min;
B:then added 4mol nickel fluoride power, controlled the mixing speed at250rpm to react for 4h, let stand for 50min, layered, washed with sodium chloride solution with a mass fraction of 21% for40min, washed with 1-pentanol solution with a mass 10 fraction of 46% for 40min, recrystallized in 2-hexone solution with a mass fraction of 65%, dehydrated with anhydrous calcium sulfate dehydration, got the finished product peroxide second tert butyl286.744g, yield of 98.2%.
The embodiment of the present invention are merely preferred embodiment of the present invention, but the range of the present invention is not limited this, and 15 any person who is familiar with those skilled in the arts, within the technical range of the present invention. It is intended that the technical solution and its inventive concept be replaced or modified equivalently with reference to the range of the invention.
Claims (5)
1. Peroxide second tert butyl organic intermediates synthesis method, comprises the following steps: A: 2-methyl-2-propylamine and potassium sulfate solution were added to the reaction vessel, controlled the mixing speed at 110-130 rpm, controlled the reaction temperature of the solution to 5-10 C, added isopropyl alcohol aluminum, added the second glycol two ethyl ether solution in batches in 30-50min, continued to react for 90-120min; B:then added nickel fluoride power, controlled the mixing speed at 220-250rpm to react for 2-4h, let stand for 30-50min, layered, washed with sodium chloride solution for30-40min, washed with 1-pentanol solution for 20-40min, recrystallized in 2-hexone solution, dehydrated with dehydration, got the finished product peroxide second tert butyl·
2. Peroxide second tert butyl organic intermediates synthesis method according to claim I wherein the potassium, sulfate solution has a mass fraction of 10-16%.
3. Peroxide second tert butyl organic intermediates synthesis method according to claim I wheiein the mass fraction of second glycol two ethyl ether solution is 20-25%.
4. Peroxide second tert butyl organic intermediates synthesis method according to claim I wherein the sodium chloride solution has a mass fraction of 15-21%.
5. Peroxide second tert butyl organic intermediates synthesis method, according to claim 1. wherein the 1-pentanol solution has amass fraction of 40-46%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IES20180255 IES87061B2 (en) | 2018-08-16 | 2018-08-16 | Peroxide second tertbutyl [Di-tert-butyl peroxide] organic intermediates synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IES20180255 IES87061B2 (en) | 2018-08-16 | 2018-08-16 | Peroxide second tertbutyl [Di-tert-butyl peroxide] organic intermediates synthesis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| IES20180255A2 IES20180255A2 (en) | 2019-10-30 |
| IES87061B2 true IES87061B2 (en) | 2019-10-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| IES20180255 IES87061B2 (en) | 2018-08-16 | 2018-08-16 | Peroxide second tertbutyl [Di-tert-butyl peroxide] organic intermediates synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| IE (1) | IES87061B2 (en) |
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2018
- 2018-08-16 IE IES20180255 patent/IES87061B2/en unknown
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| Publication number | Publication date |
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| IES20180255A2 (en) | 2019-10-30 |
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