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Propionyl-L-carnitine synthesis technology and detection method of related substance and its content

A synthesis process and technology for related substances are applied in the field of propionyl-L-carnitine synthesis process and detection of related substances and contents, which can solve the problems of heavy pollution, many by-products, and high danger for workers to operate, and achieve sensitivity. High efficiency, less by-products, safe operation

Inactive Publication Date: 2005-08-10
SUZHOU LANXITE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The synthesis method announced by British Patent 2048268A is to dissolve L-carnitine in trifluoroacetic acid, add propionyl chloride dropwise, react and filter at 40-50 degrees Celsius, and use trifluoroacetic acid as a solvent, which has high cost, heavy pollution, and dangerous operation for workers. Large, but the use of other solvents has problems such as difficulty in dissolving and many by-products, so solvent selection is the key and difficulty restricting the synthesis process
For the detection method of propionyl-L-carnitine hydrochloride (propionyl-L-carnitine chloride) and its internal salt (base) related substances and content, there is no public report yet, and the difficulty of its determination method lies in that it contains quaternary Amino groups, and at the same time have acidic groups, its ultraviolet absorption is weak at the wavelength of 200-400 nm, the peak shape and detection sensitivity are low, and the detection method and solvent selection are very difficult

Method used

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Experimental program
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Effect test

Embodiment 1

[0017] The synthesis process of propionyl-L-carnitine hydrochloride of the present invention is as follows: take 16.2 grams of L-carnitine, add 3 grams of p-toluenesulfonic acid, dry propionic acid with 40 grams, stir and dissolve, add propionyl chloride 30 gram, the temperature was raised to 45 degrees centigrade after dropping, and the insulation reaction was carried out for 20 hours. After the reaction, take it out and cool to room temperature, add 410 grams of acetone, stir for 2 hours, filter, add 490 grams of diethyl ether to the filtrate, stir until a white precipitate precipitates, and put it in the refrigerator for refrigeration. Filter and dry to obtain 22.5 g of propionyl-L-carnitine hydrochloride, with a yield of 88.2%. Dissolve it in ethanol, pass through ammonia gas for 1 hour, filter out the precipitate, add 380 g of acetone and 490 g of ether, and filter to obtain 18.3 g of propionyl-L-carnitine inner salt, with a yield of 95%.

[0018] The detection method of...

Embodiment 2

[0020] The synthesis technique of propionyl-L-carnitine hydrochloride inner salt of the present invention is as follows: get 18 grams of L-carnitine hydrochloride, add 6 gram p-toluenesulfonic acid, dry propionic acid with 60 grams, stir and dissolve, 5 grams of propionyl chloride was added dropwise, and the temperature was raised to 50 degrees Celsius after dropping, and the temperature was kept for 20 hours. After the reaction, take it out and cool to room temperature, add 390 grams of acetone, stir for 2 hours, filter, add 510 grams of diethyl ether to the filtrate, stir until a white precipitate precipitates, and put it in the refrigerator for refrigeration. Filter and dry to obtain 24.8 g of propionyl-L-carnitine hydrochloride, with a yield of 88.3%. Dissolve it in ethanol, pass through ammonia gas for 1 hour, filter out the precipitate, add 400 g of acetone and 500 g of ether, and filter to obtain 20.1 g of propionyl-L-carnitine inner salt, with a yield of 94.9%.

[002...

Embodiment 3

[0023] The synthesis process of propionyl-L-carnitine hydrochloride inner salt of the present invention is as follows: get 16 grams of L-carnitine, add 2 grams of p-toluenesulfonic acid, stir and dissolve with 40 grams of propionic acid, add propionyl chloride dropwise 30 grams, the temperature was raised to 45 degrees Celsius after dropping, and the temperature was kept for 20 hours. After the reaction, take it out and cool to room temperature, add 410 grams of acetone, stir for 2 hours, filter, add 490 grams of diethyl ether to the filtrate, stir until a white precipitate precipitates, and put it in the refrigerator for refrigeration. Filter and dry to obtain 22.1 g of propionyl-L-carnitine hydrochloride, with a yield of 88.0%. Dissolve it in ethanol, pass through ammonia gas for 1 hour, filter out the precipitate, add 380 g of acetone and 520 g of ether, and filter to obtain 18.3 g of propionyl-L-carnitine inner salt, with a yield of 95%.

[0024] The detection method of t...

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PUM

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Abstract

A process for synthesizing the propionyl-L-carnitine features the acylation reaction between L-carnitine and propionyl chloride in propionic acid as solvent under the catalysis of p-toluenesulfonic acid. The method for measuring the contents of propionyl-L-carnitine and associated substances features that the efficient liquid-phase chromatography is used to measure the content of propionyl-L-carnitine and the thin-layer chromatography is used to detect associated substances.

Description

technical field [0001] The invention relates to a synthesis process of propionyl-L-carnitine hydrochloride and its inner salt, and a detection method for related substances and content. Background technique [0002] The synthesis method announced by British Patent 2048268A is to dissolve L-carnitine in trifluoroacetic acid, add propionyl chloride dropwise, react and filter at 40-50 degrees Celsius, and use trifluoroacetic acid as a solvent, which has high cost, heavy pollution, and dangerous operation for workers. Large, but the use of other solvents has problems such as difficulty in dissolving and many by-products, so the choice of solvent is the key and difficult point restricting the synthesis process. For the detection method of propionyl-L-carnitine hydrochloride (propionyl-L-carnitine chloride) and its internal salt (base) related substances and content, there is no public report yet, and the difficulty of its determination method lies in that it contains quaternary ...

Claims

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Application Information

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IPC IPC(8): C07C227/16C07C229/22G01N30/02G01N30/90
Inventor 贡肖巍徐文芳郑家晴张建礼翟海民王丽崔美兰
Owner SUZHOU LANXITE BIOTECH
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