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Process for preparing acetyl levocarnitine hydrochlorate

A hydrochloride and acetyl technology, applied in the field of drug synthesis, can solve the problems of low quality recrystallization products, long heating time of materials, and increased side reactions, etc., to achieve both material solubility and crystallization rate, and save steps and equipment , the effect of reducing the dosage

Inactive Publication Date: 2005-01-12
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention provides a method for preparing acetyl levocarnitine hydrochloride by using levocarnitine inner salt as a starting material, which solves the problem of excessive heating time of materials in the prior art due to high reaction temperature and distillation operation process Increased side effects caused by
Simultaneously, the present invention also solves the problems of low solubility and low quality recrystallized products that exist in the prior art method with isopropanol single solvent recrystallization

Method used

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  • Process for preparing acetyl levocarnitine hydrochlorate

Examples

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Effect test

Embodiment 1

[0021] The preparation method of acetyl levocarnitine hydrochloride is in a four-necked bottle equipped with stirring, condenser and thermometer; add levocarnitine inner salt 40g (0.25mol), glacial acetic acid 48ml, stir to dissolve, add Catalyst p-dimethylaminopyridine 0.1g, maintain the external temperature at 40°C, add 26.5ml of acetyl chloride (0.375mol) dropwise, after the addition is complete, control the temperature at 40-50°C, keep the temperature for 2 hours, cool down to 0°C, and crystallize Filtrate, wash the filter cake with 25ml of isopropanol × 2, and dry to obtain 50g of crude product acetyl levocarnitine hydrochloride, then add the crude product to 150ml of isopropanol containing 10% water, stir and heat to dissolve, and wait until the solution is transparent. Add 1g of activated carbon, decolorize for 10 minutes and then filter, cool the filtrate to room temperature and then cool it to -5°C with ice-salt water, filter, wash the filter cake with 25ml of isopropa...

Embodiment 2

[0023] In the same device as Example 1, add 40 g (0.25 mol) of internal salt of levocarnitine, 60 ml of glacial acetic acid, stir and dissolve, add catalyst p-dimethylaminopyridine 0.04 g, control the internal temperature between 40-50 ° C, Add 26.5ml of acetyl chloride (0.375mol) dropwise, keep the reaction for 5 hours, then cool down to -5°C, crystallize and filter, wash the filter cake with isopropanol, 25ml×2, and dry to obtain crude acetyl-levocarnitine hydrochloride Salt 47g, then crude product is added to 140ml, in the isopropanol containing water 10%, obtain fine product acetyl levocarnitine hydrochloride 37g, content 99.4% according to embodiment 1 refining step.

Embodiment 3

[0025] In the same device as Example 1, add 40 g (0.25 mol) of internal salt of levocarnitine, 40 mL of glacial acetic acid, stir and dissolve, add catalyst p-dimethylaminopyridine 0.2 g, control the internal temperature between 10-20 ° C, Add 26.5ml of acetyl chloride (0.375mol) dropwise, after the addition is complete, keep at 10-20°C, react for 3 hours, cool to -2°C, crystallize and filter, wash the filter cake with 25ml of isopropanol × 2, and dry to obtain the crude product of acetyllevocar Nitin hydrochloride 52g, then the crude product was added in 156ml of water-containing 8% isopropanol, according to the refining steps of Example 1, 39g of refined acetyl levocarnitine hydrochloride was obtained, with a content of 98.9%.

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Abstract

The present invention belongs to the field of medicine synthesis and features that by using levocarnitine inner salt as initial material, glacial acetic acid as solvent and in the presence of catalyst, the present invention produces coarse levocarnitine hydrochloride product directly via crystal separation at relatively low temperature, and the coarse product is recrystallized to obtain the product. The process is simple and low in power consumption, and has less side reactions and high product quality.

Description

(1) Technical field [0001] The invention belongs to the field of medicine synthesis. (2) Technical background [0002] Acetyl-levocarnitine hydrochloride, also known as: acetylcarnitine hydrochloride (or acetylcarnitine hydrochloride) [0003] English name: L---Acetyl carnitine Hydrochloride [0004] Structural formula: [0005] Acetyl-levocarnitine is an endogenous substrate for the synthesis of acetylcholine in the human brain, and has neuroprotective and mitochondrial protective effects. It can actively participate in the energy metabolism of mitochondria in cells and correct the DNA transcription of mitochondria. Acetyl-L-carnitine thus prevents the aging and degenerative processes of the nervous system. Because it can stimulate nerve cells to produce protein core cell membranes and release the nerve mediator - acetylcholine, it has the effect of promoting memory improvement and improving recognition ability. Its clinical application is mostly in the form of hydroc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/16C07C229/22
Inventor 朱树森张晓杰张海燕
Owner NORTHEAST PHARMA GRP