Preparation method of sarpogrelate hydrochloride photodegradation impurities

Abstract

The invention belongs to the field of pharmaceutical synthesis and specifically relates to a preparation method of sarpogrelate hydrochloride photodegradation impurities. According to the preparation method, salicylaldehyde is used as a raw material to prepare a degradation impurity II by three steps of a substitution reaction, an addition reaction and an esterification reaction, etc., and a crude product undergoes column chromatography isolation such that purity reaches more than 99%; 2-[2-(3-methoxyphenyl)ethylene]phenol is used as a raw material to prepare a sarpogrelate hydrochloride impurity III by five steps of a substitution reaction, an addition reaction, an esterification reaction, an epoxidation reaction and a reduction reaction, etc., and a crude product undergoes column chromatography isolation such that purity reaches more than 99%; and [[2-[2-(3-methoxyphenyl)ethyl]phenoxyl]methyl]oxirane is used as a raw material to prepare a sarpogrelate hydrochloride gradation impurity IV by four steps of an addition reaction, amino protection, an esterification reaction and deprotection, etc., and a crude product undergoes column chromatography isolation such that purity reaches more than 99%. The preparation method is simple to operate, and reactions are mild. Product purity is high. The preparation method is suitable for impurity spectrum analysis. By the preparation method, overall yield is high.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and in particular relates to a preparation method for photodegrading impurities of sarcogrelate hydrochloride. Background technique [0002] Sagrelate Hydrochloride Tablets was first launched in Japan in 1993 under the trade name Anplag, which is a 5-HT2 receptor blocker that can inhibit platelet aggregation and vasoconstriction, has antithrombotic effect and improves microcirculation. Its indications are to improve ischemic symptoms such as ulcers, pain and cold sensation caused by chronic arterial occlusive disease. The sarcogrelate hydrochloride raw material drug used for the preparation of sarcogrelate hydrochloride tablets needs to meet the required purity, and the simple impurity content must also meet the corresponding requirements. In Japan's March 2012 revision of the drug instructions, the standard product classification number: 873399 specifies four photodegradable impurities of sagrelat...

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Problems solved by technology

[0004] At present, there are no literature and patent reports on the preparation method of sagrelate hydrochloride photodegradation impurities. In order to better carry out quality research on sarcogrelate hydrochloride raw materials and ensure product quality, the inventors have carried out photodegradation of sarcogrelate hydrochloride. The chemical synthesis of impurities was studied, and a preparation method of high-purity photodegradation impurities was obtained, which provided a guarantee for improving the quality of sagrelate hydrochloride raw materials

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