反应 #3247922
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08969335B2
反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Sodium hydride, 60% suspension in oil (3.6 g, 0.09 mol), is added to a solution of cyclopropylmethanol (6.49 g, 0.09 mol) in dry DMF (200 ml) at 0° C. under nitrogen. After 30 min at 0° C., 5-bromo-2-fluorobenzonitrile (12.0 g, 0.06 mol) in dry DMF (50 ml) is added, and the reaction is stirred at 50° C. for 16 h. Ice-water (200 ml) is added to the reaction mixture, which is then extracted with ethyl acetate (2×200 ml). The organic phases are washed with water (2×200 ml) and saturated sodium chloride solution (1×200 ml) and dried over sodium sulfate. After removal of the solvent, the crude product is purified by chromatography, giving 14 g of a yellow oil; is then extracted with ethyl acetate (2×200 ml) The organic phases are washed with water (2×200 ml) and saturated sodium chloride solution (1×200 ml) dried over sodium sulfate After removal of the solvent the crude product is purified by chromatography
来源 ID: ord-349699eb17d144dab713106e68d0929d