Synthesis process of thiazole medical intermediate

Abstract

The invention discloses a synthesis process of thiazole medical intermediate.The synthesis process comprises the following steps: step 1, mixing ethyl pyruvate and dichloromethane of which the volume is 2 times that of the ethyl pyruvate at room temperature, adding an obtained mixture into a reactor, starting stirring, and keeping the temperature of a system at about 20 DEG C; step 2, starting to dropwise add a dichloromethane solution of bromine, controlling the temperature to enable the system to be about 20-30 DEG C, sealing the reactor, and introducing a strong alkali solution to absorb acid gas HBr; and step 3, after dropwise adding is completed, closing a cold well, performing stirring at normal temperature for about 2 hours until the color of the reaction liquid gradually becomes light yellow to light brown, monitoring that no raw material exists through TLC, and concentrating the obtained reaction liquid. According to the synthesis process of the thiazole medical intermediate, by introducing the defoaming agent n-hexane, generated gas foam can be quickly dissolved out and released from the solvent, and the phenomenon of one-time flushing is avoided; and by introducing the n-hexane solvent, solids can be effectively separated out at low temperature, the impurity content can be controlled to be about 1%, the purification difficulty is greatly reduced, and crystallization is facilitated.

Description

technical field [0001] The invention relates to a synthesis method of thiazole, in particular to a synthesis process of a thiazole pharmaceutical intermediate, and belongs to the technical field of pyridine synthesis. Background technique [0002] Thiazole is an organic compound with a chemical formula of C3H3NS. It is a colorless or light yellow liquid with a special odor. It can be used as an organic synthesis reagent for the synthesis of drugs, dyes, rubber accelerators, film color, fungicides and dyes. At the same time, thiazole compounds have been proved to have superior pharmacological and biological activities, and have been widely used in the fields of antitumor, bactericidal and antiviral. [0003] As a key part of pharmaceutical intermediates, thiazole has rarely been able to achieve mass production in the market. The production process of thiazole is generally a diazotization reaction, and the diazotization reaction is characterized by poor production of by-produ...

AI Technical Summary

Problems solved by technology

The production process of thiazole is generally a diazotization reaction, and the diazotization reaction is characterized by poor production of by-products, difficulty in controlling the accuracy of temperature control, more gas generated in the reaction, and very easy to spray materials, resulting in the amplification of the reaction Risk, while product purification is difficult, not conducive to crystallization

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