反应详情

4-Methoxybenzylamine (0.026 ml, 0.24 mmol) and then sodium triacetoxyborohydride (0.08 g, 0.377 mmol) were added to a solution of 4-hydroxy-4-[2-(6-methoxyquinazolin-4-yl)-ethyl]cyclohexanone (0.06 g, 0.2 mmol) in dichloromethane (1 ml). The reaction mixture was stirred overnight and then filtered over Hydromatrix (wetted with an NaHCO3 solution, 2 ml) and subsequently washed with dichloromethane. The filtrate was concentrated to dryness by rotary evaporation. The residue was purified by column chromatography on silica gel (dichloromethane/MeOH 9/1 and then dichloromethane/MeOH 9/1 and 2% triethylamine).

1. filtrationfiltered over Hydromatrix (
2. washsubsequently washed with dichloromethane
3. concentrationThe filtrate was concentrated to dryness by rotary evaporation
4. customThe residue was purified by column chromatography on silica gel (dichloromethane/MeOH 9/1