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Preparation method of carbasalate calcium

A technology of calcium carbasalate and calcium nitrate, applied in the field of fine chemical product preparation, can solve the problems of high production cost, difficult removal of residues, difficult production and the like, and achieves the effects of overcoming poor safety, low production cost, and concise production process

Active Publication Date: 2009-11-11
ZHEJIANG SHENGXIAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following problems: ethylene glycol monomethyl ether is a highly toxic solvent, and long-term contact can cause irreversible damage to the hematopoietic system; ethylene glycol monomethyl ether has a high boiling point and is difficult to recycle, resulting in high production costs; Ether is easy to adsorb on the product, and the residue is not easy to remove, so it needs to be cleaned with ether, so there is a safety hazard; the yield is 74.16%, and the yield is low
There are problems in this process: acetone is flammable and explosive, and the production risk factor is high; the boiling point of acetone is low, recovery is difficult, and the production cost is high; acetone and ethanol are used as mixed solvents, and separation is difficult, causing certain difficulties to production

Method used

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Examples

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preparation example Construction

[0014] Preparation of aspirin calcium salt

[0015]

[0016] Preparation of Carboprine Calcium

Embodiment 1

[0018] (1) Pump 300kg of methanol into a 500L dissolving kettle, stir, increase the temperature to 35°C, add 50kg of aspirin, 10.5kg of urea, and 25kg of anhydrous calcium nitrate in sequence, keep it warm and stir for 40 minutes to dissolve it, press filter to 2000L In the crystallization kettle. The temperature of the crystallization kettle is cooled to 0-5°C through cooling water.

[0019] (2) Under the condition of maintaining a temperature of 0-5°C, start to pass ammonia gas and stir to make the pH value of the reaction system about 7.5, and the temperature of the reaction system does not exceed 10°C.

[0020] (3) Keep stirring, release the cooling water, add hot water around 35°C to circulate the temperature to increase the temperature in the crystallization kettle to 35°C. After keeping the crystallization for 5 hours, put the material into the centrifuge to filter and keep the centrifuge for 30 minutes.

[0021] (4) Pellet the dried material with a 12-mesh sieve, enter a d...

Embodiment 2

[0023] (1)Pump 250kg of ethanol into a 500L dissolving kettle, stir, increase the temperature to 35℃, add 50kg of aspirin, 10.5kg of urea, and 25kg of anhydrous calcium nitrate in sequence, keep it warm and stir for 40 minutes to make it completely dissolved, press filter to 2000L In the crystallization kettle. The temperature of the crystallization kettle is cooled to 0-5°C through cooling water.

[0024] (2) Under the condition that the temperature is maintained at 0-5°C, ammonia gas is introduced and stirred, so that the pH value of the reaction system is about 7.5, and the temperature of the reaction system does not exceed 10°C.

[0025] (3) Keep stirring, release the cooling water, add hot water around 35°C and circulate the temperature to increase the temperature in the crystallization kettle to 45°C. After keeping the crystallization for 5 hours, put the material into the centrifuge to filter and keep the centrifuge for 30 minutes.

[0026] (4) Pellet the dried material wit...

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Abstract

The invention discloses a preparation method of carbasalate calcium, comprising the following steps of: according to parts by weight, adding 4 to 6 parts of methanol or ethanol solvent in a dissolution kettle, heating up to 30 DEG C to 40 DEG C, adding 1 part of aspirin, 1.1 parts of urea and 1.05 parts of calcium nitrate in sequence, heating and stirring for fully dissolution, then filtering to a reaction kettle; after the filtrate is cooled to 0 DEG C to 5 DEG C, introducing an ammonia solution of the methanol or ethanol and stirring, keeping the temperature below 10 DEG C till the pH value of the reaction system reaches neutral; keeping stirring, heating up to 40 DEG C to 45 DEG C, conducting crystallization and centrifugation, drying and packaging, and then obtaining the finished product. The preparation method uses the methanol or ethanol as single solvent, solves the problems of poor safety performance, high production cost, difficult recycling of solvent and the like caused by the adoption of the mixed solvent of ethylene glycol monomethyl ether and ethanol in the prior art; the preparation method has the advantages of concise production process, low production cost and good safety performance; and the yield can reach 95 to 96 percent.

Description

【Technical Field】 [0001] The invention belongs to a method for preparing fine chemical products, in particular to a method for preparing carbopirin calcium. 【Background technique】 [0002] Carbasalate Calcium is an aspirin derivative with a chemical name of bis-(2-acetoxybenzoic acid) urea. It was first developed by the Dutch company DSM and its trade name was ASCAL. It was approved for production by the Dutch health authorities in 1974. , Currently included in the fifth edition of the European Pharmacopoeia (EP5). Because the product has high bioavailability, low side effects and good water solubility, and its curative effect is similar to aspirin, it has received wide attention and has been used in clinical practice abroad. my country began to import carbopirin calcium raw materials (import license number X900101) in 1990, which was produced by Beijing Wanhui Pharmaceutical Factory in cooperation with Dutch DSM company. The preparation variety was named Suketong (that is, carba...

Claims

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Application Information

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IPC IPC(8): C07C275/02C07C273/02C07C69/157C07C67/00
Inventor 冯永胜郭水林郭小忠
Owner ZHEJIANG SHENGXIAO CHEM
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