反应详情

To a solution of (4-amino-3′-chloro-biphenyl-3-yl)-cyclopropyl-methanone (0.67 g, 2.5 mmol) in anhydrous THF (10 mL) at −78° C. was added a solution of methylmagnesium bromide (3.0 M in diethyl ether, 2.5 mL, 7.5 mmol) under nitrogen. The reaction mixture was slowly warmed to rt, stirred under nitrogen for 12 hours, and quenched with a saturated aqueous ammonium chloride solution (40 mL). Ethyl acetate (50 mL) was added, the organic layer was separated, and dried (MgSO4). After removal of the solvent, the residue was purified via silica gel chromatography (hexane:ethyl acetate/7:1) to afford 1-(4-amino-3′-chloro-biphenyl-3-yl)-1-cyclopropyl-ethanol as yellow oil: MS (EI) m/z 287/289 (M+).

1. customquenched with a saturated aqueous ammonium chloride solution (40 mL)
2. additionEthyl acetate (50 mL) was added
3. customthe organic layer was separated
4. dry with materialdried (MgSO4)
5. customAfter removal of the solvent
6. customthe residue was purified via silica gel chromatography (hexane:ethyl acetate/7:1)