反应详情

To a solution of the intermediate isolated in Step C in 100 mL of dichloromethane was added 1.41 mL (12.0 mL) of 1-(2,4-dichlorophenyl)methanamine, followed by 2.54 g (12.0 mmol) of sodium triacetoxyborohydride, and 0.960 mL (16.0 mmol) of acetic acid. After 16 h at ambient temperature, the reaction was quenched with an equal volume of saturated aqueous NaHCO3. The mixture was extracted twice with dichloromethane, and the combined organic layers were dried (Na2SO4), and concentrated in vacuo, affording a yellow solid. Purification by flash chromatography (15% EtOAc in hexane) afforded the title compound as a white solid.

1. customthe reaction was quenched with an equal volume of saturated aqueous NaHCO3
2. extractionThe mixture was extracted twice with dichloromethane
3. dry with materialthe combined organic layers were dried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customaffording a yellow solid
6. customPurification by flash chromatography (15% EtOAc in hexane)