反应详情

To a solution of 3-cyclopropyl-4-fluoro-benzamide (Preparation 57, 66 g, 0.37 mol, 1.0 eq) in THF (500 mL) was added portionwise lithium aluminium hydride (42 g, 1.1 mol, 3.0 eq) at 10° C. Then the mixture was stirred at room temperature overnight. Water (100 mL) was added dropwise to the reaction mixture at 10° C. and the mixture was filtrated. The solid was washed with THF (3×700 mL), and filtrate was dried over sodium sulfate and concentrated in vacuum to give crude. The crude product was purified by column chromatography (MeOH/DCM 1:100→1:40) to give title compound as a yellow liquid (42.27 g, 0.257 mol, 69.5%).

1. filtrationthe mixture was filtrated
2. washThe solid was washed with THF (3×700 mL), and filtrate
3. dry with materialwas dried over sodium sulfate
4. concentrationconcentrated in vacuum
5. customto give crude
6. customThe crude product was purified by column chromatography (MeOH/DCM 1:100→1:40)