Halcinonide producing process

Abstract

The present invention is the production process of fluorizing Halcinonide with intermediate condensating and reducing as material. The technological process incldues fluorizing reaction with hydrogen fluoride and dimethyl methane amide solution, dilution with great amount of water, neutralization with ammonia water, filtering, and drying; recrystallization to refine through dissolution with mixed solvent of chloroform and methanol, concentration, addition of methanol for recrystallization; and filtering and drying to obtain the fluorized Halcinonide product. The said technological process has high yield and quality of the fluorized product.

Description

Technical field: [0001] The invention relates to a production process of fluorine on halcinonide. Background technique: [0002] The traditional fluorine-encapsulating production process of halcinonide uses halcinonide intermediate condensate as a raw material, and uses 60% hydrogen fluoride aqueous solution to carry out fluorine-reaction. After the reaction is completed, it is diluted with a large amount of water, neutralized with ammonia water, filtered, and dried; Then carry out recrystallization and refinement, dissolve with a mixed solvent of chloroform and methanol with a volume ratio of 7:3; Its shortcoming is that water is used as a solvent, the polarity of the solvent is strong, the selectivity of the reaction is not high, and the 21-position is prone to hydrolysis during the reaction process, resulting in unstable reaction and low quality and yield. [0003] Condensation compound Fluorine compound Invention content: [0004] Aiming at the existing...

AI Technical Summary

Problems solved by technology

Its shortcoming is that water is used as a solvent, the polarity of the solvent is strong, and the selectivity of the reaction is not high. During the reaction, the 21-position is prone to hydrolysis, resulting in unstable reaction and low quality and yield.