Preparation method for acetyl-L-carnitine nitrate

A technology of acetyl-L-carnitine and L-carnitine, applied in the field of preparation of acetyl-L-carnitine nitrate, can solve problems such as enhancement, and achieve the effects of reducing waste, facilitating purification and high yield

Pending Publication Date: 2014-03-26
TIANJIN TIANCHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Acetyl-L-carnitine is an important carnitine derivative used for the treatment of central nervous system diseases, metabolic diseases, dementia and brain aging. Clinical treatment experiments have been carried out in the United States, and at the same time, it can enhance the memory of normal people. Acetyl-L-carnitine nitrate is not easy to absorb moisture, has stable properties, and is more conducive to storage, transportation and preparation of solid preparations. At present, there is no acetyl-L-carnitine at home and abroad. A report on the synthesis method of carnitine nitrate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0028] ⅰ. Preparation of acetyl-L-carnitine:

[0029] a. Adding L-carnitine in the reaction vessel is a raw material, adding acetic acid is a solvent, and L-carnitine is dissolved;

[0030] b. Then add acetic anhydride and react at 30°C~80°C for 3~12 hours;

[0031] c. After the reaction is completed, distill under reduced pressure to remove the acetic acid in the solution, then add acetone to fully stir and disperse;

[0032] d. Cool down to below 5°C to crystallize, and keep warm at 0°C~5°C for more than 2 hours;

[0033] e. Suction filtration to separate the solid, and drying to obtain acetyl-L-carnitine;

[0034] ⅱ. Preparation of acetyl-L-carnitine nitrate:

[0035] a. taking the acetyl-L-carnitine gained in step i as a raw material, adding acetic acid as a solvent, and dissolving the acetyl-L-carnitine;

[0036] b. Then add nitric acid and react at 30°C~80°C for 2~5 hours;

[0037] c. After the reaction is completed, distill the acetic acid and water in the solution...

Embodiment 1

[0047] Add 96g of acetic acid into the reaction vessel, and add 32g of L-carnitine to dissolve under stirring. After completely dissolving, add 61.5g of acetic anhydride, then raise the temperature to 80°C and react at a constant temperature for 12 hours. Distill acetic acid below ℃, lower the temperature to 40℃, add 160g of acetone, fully stir and disperse for 0.5 hours, cool down to below 5℃ to crystallize, and keep warm for 2 hours between 0℃~5℃, separate by suction filtration, and wash the solid with acetone , dried in vacuum -0.09 Mpa, 80°C, and obtained 36g of finished product of acetyl-L-carnitine, with a yield of 88.9%.

[0048] Take 20.5g of the finished product of acetyl-L-carnitine and put it into the reaction container, then add 62g of acetic acid, stir to dissolve, raise the temperature to 60°C, add 14.5g of nitric acid, then raise the temperature to 80°C and react at constant temperature for 5 hours. , the temperature is below 80°C to distill off acetic acid, low...

Embodiment 2

[0050] Add 200g of acetic acid into the reaction vessel, and add 130g of L-carnitine under stirring to dissolve. After it is completely dissolved, add 166g of acetic anhydride, then raise the temperature to 30°C and react at a constant temperature for 3 hours. Remove acetic acid by distillation, lower the temperature to 40°C, add 260g of acetone, fully stir and disperse for 0.5 hours, cool down to below 5°C to crystallize, and keep warm at 0°C~5°C for 2 hours, separate by suction filtration, wash the solid with acetone, Dry at -0.09 Mpa in a vacuum at 80°C to obtain 147g of the finished product of acetyl-L-carnitine, with a yield of 89.2%.

[0051] Take 147g of the finished product of acetyl-L-carnitine and put it into the reaction container, then add 220g of acetic acid, stir to dissolve, raise the temperature to 30°C, add 105g of nitric acid, and then react at a constant temperature of 30°C for 2 hours. Distill and remove acetic acid at ℃, add 294g of acetone to fully stir a...

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Abstract

The invention discloses a preparation method for acetyl-L-carnitine nitrate, and belongs to an acyclic compound of which the carbon skeleton is substituted by oxygen atoms. The method specifically comprises the preparation of acetyl-L-carnitine and the preparation of the acetyl-L-carnitine nitrate. According to the technical scheme, the method is simple, easy, low in cost and favorable for industrial large-scale production; the use of a catalyst during reaction is avoided, so that purification is facilitated; the method is short in reaction time and high in production efficiency; acetic acid can be recovered by adding acetone for crystallization after being evaporated under reduced pressure after reaction, and the acetone can also be recovered in a distillation way, so that the waste of a solvent is greatly reduced, and the cost is lowered; a product is qualified and high in yield.

Description

technical field [0001] The invention belongs to an acyclic compound whose carbon frame is replaced by an oxygen atom, and in particular relates to a preparation method of acetyl-L-carnitine nitrate. Background technique [0002] There have been many reports on the efficacy of L-carnitine. It is an important food nutrition fortifier and has been widely used in the food industry, such as infant milk powder, diet food, athlete nutrition and nutritional supplements for middle-aged and elderly people, as well as feed processing industry Among them, there are also medical effects. Cardiovascular disease, liver disease, kidney disease, hyperlipidemia, diabetes, neuromuscular disease, etc. can all be improved by taking L-carnitine series of new products. [0003] Acetyl-L-carnitine is an important carnitine derivative used for the treatment of central nervous system diseases, metabolic diseases, dementia and brain aging. Clinical treatment experiments have been carried out in the U...

Claims

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Application Information

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IPC IPC(8): C07C229/22C07C227/18C07C227/16
CPCC07C229/22C07C227/16C07C227/42
Inventor 张国基
Owner TIANJIN TIANCHENG PHARMA
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