129846-94-2Relevant articles and documents
New process for preparing metopimazine
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Paragraph 0047; 0048; 0056, (2019/01/14)
The invention discloses a new process for preparing metopimazine. The new process comprises the following steps: in a reactor, using o-fluorothiophenol and 1-chloro-4-(methylsulphonyl)-2-nitrobenzeneas raw materials to react in acetone to obtain 2-(2-fluorophenyl thio)-5-(methylsulfonyl) nitrobenzene; then adding ethanol and ferric chloride for a heating reaction to generate 2-(2-fluorophenyl thio)-5-(methylsulfonyl) aniline; adding dimethyl sulfoxide, adding NaH, heating for reaction, cooling to a room temperature, adding water, and stirring to prepare 2-methylsulfonyl-10H-phenothiazine; then adding 10-acetyl-2-methylsulfoxide-10H phenothiazine and potassium hydroxide to react to prepare 10-acetyl-2-methylsulfonyl-(5-sulfoxide)-10H phenothiazine; adding acetone, carrying out concentration and extraction to obtain a methylene chloride solution of 10-acetyl-2-methylsulfonyl-10H phenothiazine; adding piperidine-4-formamide after the temperature is lowered; adding sodium borohydride acetate; carrying out reaction and filtration; and pulping filter cakes to obtain metopimazine. According to the new process provided by the invention, the final yield is greatly improved by optimizing the reaction route and reaction conditions, and the product purity reaches 99.3% or higher.