Guo Xiang-li
2013
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Journal
Journal of Hebei University of Technology
Abstract
(Chloromethyl)bis(4-fluorophenyl)methylsilane is the intermediate of fungicide flusilazole.The study can provide the basis for its industrialized production,and thereby reducing the production costs(improve intermediate purity).It was synthesized by a Grignard reagent which was prepared from 1-bromo-4-fluorobenzene and dichloro(chloromethyl)methylsilane.The reaction mixture was mixed with hydrochloric acid(5% HCl) at 0 ~ 5 ℃,after separating the organic phase,the solvent was removed under reduced pressure to give a colourless liquid,the remaining oily residue was distilled to give a pale yellow crystalline solid,the purity is more than 96% and the yield was about 88.7%.The structure of the product was characterized by 1HNMR.By control of the amount of the magnesium and the reaction temperature,the synthesis controlled the generation of impurities of the Grignard reagent,reduced the temperature of the substitution reaction and adjusted the molar ratio of silane and Grignard reagent to improve the purity of intermediates.It is a simple experimental operation with high yield and purity.Therefore,it is an effective industrial method for synthesis of(Chloromethyl)bis(4-fluorophenyl)methylsilane.