Water → (3-Cyclopropyl-4-fluorophenyl)methanamine

反応式

[CH:1]1([C:4]2[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=2[F:13])[C:7]([NH2:9])=O)[CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>C1COCC1>[CH:1]1([C:4]2[CH:5]=[C:6]([CH2:7][NH2:9])[CH:10]=[CH:11][C:12]=2[F:13])[CH2:3][CH2:2]1

参加物

実験手順

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%).