Continuous synthesis method of trimethylsilyl azide

Abstract

The invention provides a continuous synthesis method of trimethylsilyl azide. The continuous synthesis method comprises: under a protective atmosphere, continuously transporting trimethylchlorosilane and azide as reaction raw materials to a continuous synthesis device for nucleophilic substitution reaction to obtain trimethylsilyl azide , and trimethylsilyl azide is discharged continuously, and the protective atmosphere is selected from nitrogen and / or inert gas. The trimethylsilyl azide is synthesized by a continuous synthesis process, the reaction time required for the whole reaction process is short, the output is large, and the product performance is stable. At the same time, since the application adopts a continuous synthesis process, the heat of reaction can be taken away from the continuous synthesis device at any time, which is beneficial to reduce the risk of heat accumulation during scale-up reactions, simplify operations, and improve the safety of continuous batch production. Therefore, the preparation of trimethylsilyl azide by the continuous synthesis process provided by this application is beneficial to improve the safety of the entire reaction process and the quality of the product.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a continuous synthesis method of trimethylsilyl azide. Background technique [0002] Trimethylsilyl azide is a very important intermediate in organic synthesis, widely used in the synthesis of amination reagents, azidation reagents and nitrogen heterocyclic compounds. [0003] The existing literature provides a preparation method of trimethylsilyl azide, the preparation method comprising: using decahydronaphthalene as a solvent, adding trimethylchlorosilane and sodium azide to ion exchange under the condition of 60°C The reaction was carried out in resin XAD-4 to obtain the product trimethylsilyl azide. In this reaction, the yield of trimethylsilyl azide is relatively low, only 82%. [0004] Another existing document reports a preparation method of trimethylsilyl azide, which preparation method comprises: using trimethylchlorosilane and sodium azide as raw materials, and using ...

AI Technical Summary

Problems solved by technology

[0007] The main purpose of the present invention is to provide a continuous synthesis method of trimethylsilyl azide, so as to solve the problem that the existing synthesis methods are all batch reactions and have unstable product quality and poor reaction safety.