A kind of preparation method of trifluoromethyl (trimethyl) silane

Abstract

The invention provides a preparation method of trifluoromethyl (trimethyl) silane, comprising: trifluoromethanesulfonyl chloride and trimethyl silane initiate a free radical coupling reaction under the action of light or a free radical initiator to obtain trifluoromethyl silane Methyl(trimethyl)silane. The present invention uses trifluoromethanesulfonyl chloride and trimethylsilane as starting materials, undergoes a free radical coupling reaction under the action of light or a free radical initiator, to obtain trifluoromethyl (trimethyl) silane, and the reaction technology of each step is mature , conventional raw materials, mild reaction conditions, is an advantageous technical route. Experimental results show that the total yield of trifluoromethyl (trimethyl) silane product is above 80%, and the purity is above 99%.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of trifluoromethyl (trimethyl) silane. Background technique [0002] Trifluoromethyl(trimethyl)silane is a very important organic intermediate with a wide range of uses. Trifluoromethyl (trimethyl) silane can prepare many kinds of compounds containing trifluoromethyl, such as halogens, boronic acid substituted aromatic rings, and even no substitution reactions to generate corresponding trifluoromethyl substituted aromatic ring derivatives; Reaction to generate trifluoromethyl alkyne; addition to ketones to form trifluoromethyl tertiary alcohols; reaction with esters to generate trifluoromethyl ketones; reaction with heterocycles to generate trifluoromethyl-containing heterocyclic compounds, etc. [0003] The main process route of the synthetic trifluoromethyl (trimethyl) silane disclosed in the prior art is mainly as follows: Document (Tetrahedron Let...

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Problems solved by technology

[0003] The main process route of the synthetic trifluoromethyl (trimethyl) silane disclosed in the prior art is mainly as follows: Document (Tetrahedron Letters, Vol.25, No.21, pp 2195-2198, 1984) (Journalof FluorineChemistry; vol.42 (1989); p.429-434) At present, the method of synthesizing trifluoromethyl (trimethyl) silane is mainly through trifluoromethyl bromide or trifluoromethyl iodide in various reducing agents such as TADE, P(NEt 2 ) 3 It is prepared by reacting with trimethylchlorosilane in the presence of it. It is obvious that the preparation of trifluoromethyl (trimethyl)silane according to the existing route is not less than two-step reaction, the preparation is expensive, the preparation process is complicated, and it lacks effectiveness

[0004] Chinese patent (CN106117258) uses fluoroform as raw material to react with prepared potassium hexamethyldisilazane, and then reacts with trimethylchlorosilane to prepare trifluoromethyl (trimethyl) silane, which requires anhydrous Oxygen-free, ultra-low temperature reaction, high equipment requirements, complicated operation, expensive reaction reagents, not suitable for industrial scale-up

Literature (TtrrohedronLcrrers.Vol.3s.No.46, pp.8623-8624, 1994) needs to use electrolysis reaction, equipment investment is big, technology is complicated, and there is no industrial large-scale production report literature (Beckers, H.; Buerger, H. ; Bursch, P.; Ruppert, I.; Journal of Organometallic Chemistry; vol. 316; (1986); p.41-50) Grignard reagent method, which requires strict anhydrous and oxygen-free reaction, complex operation and high risk

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