反应详情

温度

0 °C

To a solution of 1-allyl-3-ethyl-3-(3-methoxy-phenyl)-azepan-2-one (as described above in Step A) (0.83 g, 2.89 mmol) in THF (20 mL) at 0° C. was added BH3.THF (1M, 2.85 mL, 2.89 mmol) with stirring. After 1 hr at 25° C. the reaction mixture was cooled to 0° C. and EtOH (5 mL), 1M NaOH (5 mL), and 30% H2O2 (10 mL) were added. The reaction mixture was stirred for 1 hr at 25° C. The solvents were removed in vacuo and the residue was partitioned between EtOAc and saturated NaHCO3 solution. The organic layer was washed with brine and dried (MgSO4), the solvents removed in vacuo and the crude product chromatographed on silica gel with hexane and ethyl acetate 1:1 to obtain the title compound.

1. stirringThe reaction mixture was stirred for 1 hr at 25° C
2. customThe solvents were removed in vacuo
3. customthe residue was partitioned between EtOAc and saturated NaHCO3 solution
4. washThe organic layer was washed with brine
5. dry with materialdried (MgSO4)
6. customthe solvents removed in vacuo
7. customthe crude product chromatographed on silica gel with hexane and ethyl acetate 1:1