反应详情

A solution of 3-chloro-5-methoxybenzylamine (4.6 mmol, 0.792 g) in DCM (anhydrous, 20 ml) was cooled to −78° C. and BBr3 (1 M in DCM, 9.43 mmol) was added dropwise. The reaction was allowed to reach room temperature over night with stirring. The reaction was quenched by careful addition of methanol (5 ml), solvents were evaporated under reduced pressure and the residue was purified by means of chromatography (silica, DCM/MeOH/NH3 (30% in water) Sep. 1, 2001 v/v/v) to provide the title compound (0.48 g, 66%) as a white solid. (DMSO, 500 MHz) δ 3.61 (s, 2H), 4.57 (br, 1H), 6.62 (s, 1H), 6.80 (s, 1H) and 6.83 (s, 1H).

1. waitto reach room temperature over night
2. customThe reaction was quenched by careful addition of methanol (5 ml), solvents
3. customwere evaporated under reduced pressure
4. customthe residue was purified by means of chromatography (silica, DCM/MeOH/NH3 (30% in water) Sep. 1, 2001 v/v/v)