Preparation method of carbasalate calcium

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 carbasalate calcium. 【Background technique】 [0002] Carbasalate Calcium is an aspirin derivative with a chemical name of bis-(2-acetoxybenzoic acid) urea. It was first successfully developed by DSM in the Netherlands. Its trade name is ASCAL. It was approved for production by the Dutch health authority in 1974. , has been included in the fifth edition of the European Pharmacopoeia (EP5). Due to its high bioavailability, few side effects, good water solubility, and curative effect similar to that of aspirin, the product has received extensive attention and has been used clinically abroad. my country began to import carbasalate calcium raw materials (import license number X900101) in 1990, which was jointly produced by Beijing Wanhui Pharmaceutical Factory and Dutch DSM company. [0003] Before the present invention is made, known technolo...

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

Images