RU2015153332A - METHOD FOR PRODUCING BIOLOGICALLY ACTIVE SUBSTANCE β-CHLORO-L-ALANINE - Google Patents

METHOD FOR PRODUCING BIOLOGICALLY ACTIVE SUBSTANCE β-CHLORO-L-ALANINE Download PDF

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Publication number
RU2015153332A
RU2015153332A RU2015153332A RU2015153332A RU2015153332A RU 2015153332 A RU2015153332 A RU 2015153332A RU 2015153332 A RU2015153332 A RU 2015153332A RU 2015153332 A RU2015153332 A RU 2015153332A RU 2015153332 A RU2015153332 A RU 2015153332A
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Prior art keywords
solution
chloro
dried
alanine
added
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RU2015153332A
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Russian (ru)
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RU2633542C2 (en
Inventor
Павел Аркадьевич Полубояринов
Геннадий Иванович Шаронов
Петр Петрович Лещенко
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Федеральное государственное бюджетное образовательное учреждение высшего образования "Пензенский государственный университет архитектуры и строительства"
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Priority to RU2015153332A priority Critical patent/RU2633542C2/en
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/17—Amino acids, peptides or proteins
    • A23L33/175—Amino acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Claims (1)

Способ получения биологически активного вещества β-хлор-L-аланина, заключающийся в том, что 5 г L-серина добавляют к 25 мл диоксана, высушенного над молекулярным ситом 3А или 4А в трехгорлой колбе, высушенный двукратным пропусканием через концентрированную серную кислоту хлористый водород вводят в раствор с перемешиванием, при насыщении раствора хлористым водородом температура повышается до 35-37°С, а затем снижается до 30°С, хлористый водород добавляют еще в течение 30 мин, к полученному раствору в течение 30 мин добавляют 2,5 г хлористого тионила и перемешивают в течение 3-4 ч при температуре 60-65°С, раствор охлаждают до 5-10°С и образовавшийся осадок β-хлор-L-аланина гидрохлорида высушивают на воронке Бюхнера с использованием водоструйного насоса, промывают 10 мл диоксана и снова высушивают, полученный β-хлор-L-аланина гидрохлорид растворяют в 15-20 мл дистиллированной воде, добавляют 2-3 мл концентрированной соляной кислоты, 0,2-0,3 г активированного угля, тщательно перемешивают, фильтруют, затем к полученному раствору добавляют насыщенный раствор гидроксида лития, доводят до pH 5,5 и охлаждают до 0-5°С, к охлажденному раствору постепенно добавляют 45-50 мл охлажденного ацетона и оставляют раствор при температуре 0-5°С в течение 1-2 ч, выпавшие кристаллы промывают охлажденным ацетоном на воронке Бюхнера и высушивают при температуре 50-60°С.The method of obtaining the biologically active substance β-chloro-L-alanine, which consists in the fact that 5 g of L-serine is added to 25 ml of dioxane dried over a molecular sieve 3A or 4A in a three-necked flask, dried by passing twice through concentrated sulfuric acid, hydrogen chloride is introduced to the solution with stirring, when the solution is saturated with hydrogen chloride, the temperature rises to 35-37 ° C, and then decreases to 30 ° C, hydrogen chloride is added for another 30 minutes, 2.5 g of thionyl chloride are added to the resulting solution over 30 minutes and stirred for 3-4 hours at a temperature of 60-65 ° C, the solution was cooled to 5-10 ° C and the precipitate of β-chloro-L-alanine hydrochloride formed was dried on a Buchner funnel using a water-jet pump, washed with 10 ml of dioxane and again dried, the obtained β-chloro-L-alanine hydrochloride is dissolved in 15-20 ml of distilled water, add 2-3 ml of concentrated hydrochloric acid, 0.2-0.3 g of activated carbon, mix thoroughly, filter, then add to the resulting solution saturated lithium hydroxide solution, adjusted to pH 5.5 and cooling t to 0-5 ° C, 45-50 ml of chilled acetone are gradually added to the cooled solution and the solution is left at a temperature of 0-5 ° C for 1-2 hours, the precipitated crystals are washed with cooled acetone on a Buchner funnel and dried at a temperature of 50- 60 ° C.
RU2015153332A 2015-12-11 2015-12-11 Method for production of biologically active substance beta-chlorine -l-alanine RU2633542C2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
RU2015153332A RU2633542C2 (en) 2015-12-11 2015-12-11 Method for production of biologically active substance beta-chlorine -l-alanine

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Application Number Priority Date Filing Date Title
RU2015153332A RU2633542C2 (en) 2015-12-11 2015-12-11 Method for production of biologically active substance beta-chlorine -l-alanine

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RU2015153332A true RU2015153332A (en) 2017-06-16
RU2633542C2 RU2633542C2 (en) 2017-10-13

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111018728A (en) * 2019-12-27 2020-04-17 暨南大学 Method and device for preparing 3-chloro-alanine hydrochloride by using water as auxiliary agent

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT1151407B (en) * 1981-05-18 1986-12-17 Mitsui Toatsu Chemicals BETA-CHLOROALANINE PREPARATION PROCESS
ES2207019T3 (en) * 1997-12-27 2004-05-16 Kaneka Corporation PROCEDURE TO PRODUCE BETA-HALOGEN-ALFA-AMINO-CARBOXYLIC ACIDS AND DERIVATIVES OF PHENYLCISTEINE AND INTERMEDIATE PRODUCTS OF THEM.
RU2537166C1 (en) * 2013-05-24 2014-12-27 Павел Аркадьевич Полубояринов Method of production of biologically active substance-selenocystine

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111018728A (en) * 2019-12-27 2020-04-17 暨南大学 Method and device for preparing 3-chloro-alanine hydrochloride by using water as auxiliary agent

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Effective date: 20171212