SU515744A1 - "Method for isolating 2-hydroxy-3-methyl-4- - Google Patents
"Method for isolating 2-hydroxy-3-methyl-4-Info
- Publication number
- SU515744A1 SU515744A1 SU1810644A SU1810644A SU515744A1 SU 515744 A1 SU515744 A1 SU 515744A1 SU 1810644 A SU1810644 A SU 1810644A SU 1810644 A SU1810644 A SU 1810644A SU 515744 A1 SU515744 A1 SU 515744A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- isolating
- hydroxy
- methyl
- maltol
- extract
- Prior art date
Links
- 238000000034 method Methods 0.000 title description 5
- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 description 12
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 description 6
- 229940043353 maltol Drugs 0.000 description 6
- 239000004952 Polyamide Substances 0.000 description 5
- 229920002647 polyamide Polymers 0.000 description 5
- 239000006286 aqueous extract Substances 0.000 description 4
- 239000002594 sorbent Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 1
- 241000218642 Abies Species 0.000 description 1
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- WSWCOQWTEOXDQX-MQQKCMAXSA-N sorbic acid group Chemical group C(\C=C\C=C\C)(=O)O WSWCOQWTEOXDQX-MQQKCMAXSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Изобретение относитс к усовершенствованию способа выделенн из пнхтовой хвои 2метил-З-окси-4-niipoHa (мальтол), ценного стабилизатора ароматических запахов в пищевой и парфюмерной промышлеикости.The invention relates to the improvement of the method of isolated from the needles of 2methyl-3-hydroxy-4-niipoHa (maltol) needles, a valuable aromatic odor stabilizer in the food and perfume industry.
Содержание мальтов в хвое достигает 1%.The content of malts in needles reaches 1%.
Известно, что экстракцн мальтола нз водных выт жек ХВОИ пихтовых пород трудоемка и многостадийна. Использование дл этой цели легколетучих, пожароопасных (диэтиловый эфир, ЭТИЛОВЫЙ спирт) и дорогосто щих (хлороформ ) органических растворителей создает трудности дл промышленной реализации процесса .It is known that the extraction of maltol from the water extracts of the NEEDLED fir trees is laborious and multistage. The use of volatile, flammable (diethyl ether, ethyl alcohol) and expensive (chloroform) organic solvents for this purpose creates difficulties for the industrial implementation of the process.
С целью упрощени процесса выделени мальтола из пихтовой хвок и получени целевого продукта ВЫСОКОЙ степени чистоты предлагаЕОт проводить экстракцию измельченного сырь (пихтовой хвои) гор чей водой и пропускать охлажденный экстракт через полиамидный сорбент. При этом происходит очистка раствора, и после упаривани водного элюата из него выпадает кр;1сталлический осадок мaльтOvTa.In order to simplify the process of isolating maltol from fir twig and obtaining the target product of HIGH purity, it is proposed to extract the crushed raw material (fir needle) with hot water and pass the cooled extract through a polyamide sorbent. When this occurs, the solution is purified, and after evaporation of the aqueous eluate, the crcc is precipitated from it; 1 the sediment of maltOvTa.
Пример 1. 0,2 кг ПИХТОВОЙ ланки с влажкостью 34% экстрагируют 1 л гор чей воды (90-95°С) и настаивают в течение 1 час. Экстракцию повтор ют дважды и объединенный буро-коричневый водный экстракт пропускают через колонку. (60X400 мм) с полиамидным сорбентом (70 г полиамидного порошка ). При этом на сорбенте оседают механические примеси и сорби ПЮтс окрашивающие вещест; а феиольного характера. Мальтол элюируетс вместе с водой. Во.чпый экстракт выпаривают до 1/10 псрвоиа-.альг.ого объема, и при сто пии В течение 36--48 час из концентрированного элюата выпадает кристаллический осадок мальтола.Example 1. 0.2 kg of OIL Lanka with a moisture content of 34% is extracted with 1 l of hot water (90-95 ° C) and infused for 1 hour. The extraction is repeated twice and the combined brown-brown aqueous extract is passed through a column. (60X400 mm) with polyamide sorbent (70 g of polyamide powder). At the same time, mechanical impurities and sorbic PUTS staining substances are deposited on the sorbent; and fayolnogo character. Maltol is eluted with water. The second extract is evaporated to 1/10 of the pseudoalgic volume, and at the stage of the crystalline maltol precipitates from the concentrated eluate for 36--48 hours.
Выход 0,39 г 0,29% от пихтовой лапки (в пересчете па абсолютно сухой вес).The output of 0.39 g of 0.29% of the fir foot (in terms of PA absolutely dry weight).
Мальт - светло-кремовый порошок с т. пл. 148-150-С сублцмпруетс при UOC.Malta - light cream powder with t. Pl. 148-150-C is sub-sampled at UOC.
Строение мальтоз по.дтверждено данным и ПМР-снектроскопней.The structure of maltose is according to data and PMR spectroscopy.
Пример 2. 25 кг пихтовой лапки с влажностью 48% экстрагируют по примеру 1.Example 2. 25 kg fir foot with a humidity of 48% is extracted according to example 1.
Водный экстракт (100 л) пропускают через колонку (80X900 мм) с 500 г полиамидного сорбента. Водный экстракт паривают до 1/20 первоначального объема.The aqueous extract (100 l) is passed through a column (80 x 900 mm) with 500 g of polyamide sorbent. Aqueous extract soar to 1/20 of the original volume.
Выход кристалл11-.е:кого мальтола составл ет 110 г или 0,6% от сырь .The yield of crystal 11-e: whom maltol is 110 g or 0.6% of the raw material.
Степень чистоты по данным флуоресцентного анализа 97%; т. пл. 152--155СThe degree of purity according to fluorescence analysis of 97%; m.p. 152--155С
Форм у;; а и з о Ci 1,1 е т с п и Form y ;; a and z o Ci 1,1 e t with p and
Способ Быдел-ени 2-мет1:л-3-окси-4-пироца, отличающийс тем, что, с целью повышени выхода и чистоты целевого продукта, водный экстракт продукта хроматографируют на полиамидном сообенте.The method of isolating 2-met1: l-3-hydroxy-4-pyrocene, characterized in that, in order to increase the yield and purity of the target product, the aqueous extract of the product is chromatographed on a polyamide link.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU1810644A SU515744A1 (en) | 1972-07-11 | 1972-07-11 | "Method for isolating 2-hydroxy-3-methyl-4- |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU1810644A SU515744A1 (en) | 1972-07-11 | 1972-07-11 | "Method for isolating 2-hydroxy-3-methyl-4- |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU515744A1 true SU515744A1 (en) | 1976-05-30 |
Family
ID=20521904
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU1810644A SU515744A1 (en) | 1972-07-11 | 1972-07-11 | "Method for isolating 2-hydroxy-3-methyl-4- |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU515744A1 (en) |
-
1972
- 1972-07-11 SU SU1810644A patent/SU515744A1/en active
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