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Refining method of acipimox

A refining method, the technology of acipimox, which is applied in the field of acipimox refining, can solve the problems of low purity of acipimox, and achieve the effect of simple post-processing, low boiling point and saving production cost

Active Publication Date: 2014-07-16
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of acipimox obtained by the above-mentioned refining method is not high, and it is difficult to be directly used in the preparation of preparations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 40ml of water to 20g of acipimox crude product, heat to 80°C, stir to dissolve, add 0.6g of activated carbon and continue to insulate and stir for 60 minutes, then filter with suction; cool the filtrate to 40°C at 40°C / h, and then add dropwise After dropping 30g of acetone, cool down to -5°C at 30°C / h to crystallize for 4h, filter with suction, wash the filter cake with 10ml of acetone, and dry (0.01MPa, 80°C) to obtain off-white acipimox. The rate is 76.5%. The content is 99.6%, the content of 5-methylpyrazine-2-carboxylic acid is 0.11%, and the maximum other impurities are 0.04%.

Embodiment 2

[0023] Add 88ml of water to 40g of crude acipimox, heat to 85°C, stir to dissolve, add 2.4g of activated carbon and continue to insulate and stir for 50 minutes, then filter with suction; cool the filtrate to 45°C at 30°C / h, and then add dropwise After dropping 50g of acetone, cool down at 20°C / h to -2°C to crystallize for 5h, filter with suction, wash the filter cake with acetone, and dry (0.01MPa, 80°C) to obtain off-white acipimox. was 87.3%. The content is 99.6%, the content of 5-methylpyrazine-2-carboxylic acid is 0.16%, and the maximum other impurities are 0.06%.

Embodiment 3

[0025] Add 125ml of water to 50g of acipimox crude product, heat to 90°C, stir to dissolve, add 2.5g of activated carbon and continue to insulate and stir for 30 minutes, then filter with suction; cool the filtrate to 50°C at 20°C / h, and then add dropwise After dropping 125g of acetone, drop the temperature to 0°C and crystallize at 5°C / h for 6h, filter with suction, wash the filter cake with acetone, and dry (0.01MPa, 80°C) to obtain off-white acipimox. The yield is 88.6%. The content is 99.8%, the content of 5-methylpyrazine-2-carboxylic acid is 0.11%, and the maximum other impurities are 0.03%.

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Abstract

The invention belongs to the field of medicine synthesis, and particularly relates to a refining method of acipimox. The acipimox is refined by adopting a method of dissolving in hot water, removing impurities by active carbon, and dropping acetone to perform secondary cooling and re-crystallization under the condition of controlling the cooling speed. According to the technical scheme, through controlling crystallization conditions, the acipimox which is higher in purity, smaller in maximum individual impurity, slighter in color and suitable for preparation can be obtained through once refining. The refining method has the advantages of simplicity and convenience in operation, high yield and low cost, and is beneficial to industrialized production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for refining acipimox. Background technique [0002] Acipimox, the chemical name is 5-methylpyrazine-2-carboxylate-4-oxide, is an anti-lipidification lipid-lowering drug, developed by Pifzer Company of the United States, and was first introduced in Italy in 1985. listed. Its functions are as follows: ①Inhibit the release of free fatty acids from the adipose tissue of the whole body, reduce the raw materials for the synthesis of cholesterol and triglycerides, thereby reducing the contents of plasma total cholesterol, triglycerides, low-density lipoproteins, and very low-density lipoproteins. ②Increase the content of high-density lipoprotein in plasma, which is beneficial to the transport and removal of cholesterol. ③ Increase liver glycogen synthesis, reduce blood sugar content, and promote fatty acid decomposition to maintain blood sugar, thereby reducing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/24
CPCC07D241/24
Inventor 赵志全提文利赵桂芳
Owner SHANDONG NEWTIME PHARMA
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