4-氯-2-三氟甲基苯乙腈

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred and ice-cooled solution of 1-azido-4-methoxy-benzene (0.500 g, 3.3523 mmol) and 4-chloro-2-(trifluoromethyl)phenylacetonitrile (1.104 g, 5.0284 mmol) in absolute ethanol (15 ml), an ice-cooled solution of sodium methoxide (0.217 g, 4.0228 mmol) in absolute ethanol (8 ml) is added drop-wise. The resulting reaction mixture is evaporated and the residue is dissolved in methylene chloride and washed with water, brine, dried over MgSO4, filtered and evaporated to afford ˜1.25 g of crude material as brownish solid. This material is purified by crystallization from methylene chloride and petroleum ether, to obtain the title compound as brown solid (1.05 g, 83% yield). M.p. 159.2-160.2° C. LC-ESI-HRMS of [M+H]+ shows 369.0712 Da. Calc. 369.072998 Da, dev. −4.9 ppm. is added drop-wise The resulting reaction mixture is evaporated the residue is dissolved in methylene chloride washed with water, brine dried over MgSO4 filtered evaporated to afford ˜1.25 g of crude material as brownish solid This material is purified by crystallization from methylene chloride and petroleum ether