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Method for synthesizing propionyl levo-carnitine hydrochlorate

A technology for synthesizing propionyl-L-carnitine and propionyl-L-carnitine, which is applied in the field of synthesis of aminocarboxylic acid compounds, can solve the problems of unsafe hazard, low boiling point of diethyl ether, waste of solvent and the like, so as to improve production efficiency and reduce solvent waste and cost savings

Active Publication Date: 2012-12-12
リャオニンコンセプヌトラシーオーエルティーディー
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the solvent is changed to propionic acid, which reduces the toxicity, but a large amount of acetone and ether are used in the crystallization, which wastes solvents, and the boiling point of ether is low, which is likely to bring unsafe hidden dangers in industrial production.

Method used

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  • Method for synthesizing propionyl levo-carnitine hydrochlorate
  • Method for synthesizing propionyl levo-carnitine hydrochlorate

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 600g of propionic acid weighed into the reaction tank (1L), add 300g of L-carnitine inner salt under stirring to dissolve, after completely dissolving, add 207g of propionyl chloride dropwise; then raise the temperature to 70°C and keep the temperature for 2 hours; distill and concentrate under reduced pressure To crystallization, cool down and add 400g of acetone, fully stir and disperse for 0.5 hours, cool down and crystallize, and keep warm at 0-5°C for 2 hours; filter, wash the material with acetone, and suction filter to obtain the crude propionyl-L-carnitine hydrochloride. Vacuum -0.09Mpa and dry at 80°C. 427.8 g of the crude product was obtained with a yield of 96.3%.

[0032] Take 300 g of the dried crude product propionyl-L-carnitine hydrochloride, add it into a reactor containing 600 g of absolute ethanol and stir to dissolve; heat up to 50°C, and keep the temperature constant for 0.5 hours to ensure sufficient dissolution; Concentrate by pressure distill...

Embodiment 2

[0040] Add 600g of propionic acid that has been weighed into the reaction tank, add 300g of L-carnitine inner salt under stirring to dissolve, and after it is completely dissolved, add 207g of propionyl chloride dropwise; then raise the temperature to 70°C and keep the temperature for 6 hours; distill under reduced pressure and concentrate until crystallization , add 500g of acetone at lower temperature, fully stir and disperse for 0.5 hours, lower the temperature and crystallize, and keep warm at 0-5°C for 2 hours; filter and suction filter to obtain crude propionyl-L-carnitine hydrochloride, and dry at 80°C with vacuum -0.09Mpa 449.1 g of crude product was obtained with a yield of 95.2%.

[0041] Take 300 g of the dried crude product propionyl-L-carnitine hydrochloride, add it into a reactor containing 600 g of absolute ethanol and stir to dissolve; heat up to 50°C, and keep the temperature constant for 0.5 hours to ensure sufficient dissolution; Concentrate by pressure dist...

Embodiment 3

[0043]Add 15kg of propionic acid that has been weighed into the reaction tank, add 10kg of L-carnitine inner salt under stirring to dissolve, and after it is completely dissolved, add 7.2kg of propionyl chloride dropwise; then raise the temperature to 70°C and keep the temperature for 6 hours; crystallization, add 24kg of acetone at lower temperature, fully stir and disperse for 1 hour, lower the temperature to crystallize, and keep warm for 2 hours at 0-5°C; 0.09Mpa was dried at 80°C to obtain 451.5g, with a yield of 95.7%.

[0044] Take 30kg of the dried crude product propionyl-L-carnitine hydrochloride, add it into a reactor filled with 60kg of absolute ethanol and stir to dissolve; heat up to 50°C and keep the temperature constant for 1 hour to ensure sufficient dissolution; Concentrate by pressure distillation, evaporate about 40kg of ethanol, then drop to 40°C, add 50kg of acetone to stir and disperse, cool down to 0-10°C for crystallization for 1 hour; then filter, spin...

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Abstract

The invention discloses a new synthesizing method of propionyl left-handed carnitine hydrochlorate, which comprises the following steps: 1. adopting inner salt of left-handed carnitine as raw material and propionic acid as solvent; adding propionyl chloride; heating to react; decompressing to evaporate propionic acid; adding acetone; stirring to disperse; cooling to evolve; sucking; drying to obtain rough product; 2. heating to dissolve rough product through alcohol or carbinol; sucking the filtrate; decompressing; distilling to condense; evaporating partial alcohol or carbinol; cooling; adding acetone to stir evenly; cooling to evolve; filtering; drying; obtaining the pure product.

Description

technical field [0001] The invention relates to a method for synthesizing aminocarboxylic acid compounds, in particular to a method for synthesizing propionyl-L-carnitine hydrochloride, which belongs to the preparation technology of pharmaceutical intermediates and food additives. Background technique [0002] There have been many reports on the efficacy of L-carnitine (L-carnitine, L-carnitine). L-carnitine is an important food nutrition enhancer and has been widely used in the food industry, such as baby milk powder, diet food, athletes Nutritional products and nutritional supplements for middle-aged and elderly people, as well as in the feed processing industry, in addition to medical effects, cardiovascular diseases, liver diseases, kidney diseases, hyperlipidemia, diabetes, neuromuscular diseases, etc. can all be treated by taking L-meat Alkaline series of new products have improved symptoms, and it has been reported that L-carnitine can also improve reproductive capaci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/22C07C227/16
Inventor 袁学亮梅国庆卿笃清关秋陈泠
Owner リャオニンコンセプヌトラシーオーエルティーディー
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