反应详情

温度

25 °C

To a solution of 3-ethyl-3-(3-benzyloxy-phenyl)-azepan-2-one, as described above in Step A, (1.65 g, 5.1 mmol) in DMF (25 mL) at 0° C. was added NaH (0.265 g, 6.63 mmol) and the mixture was stirred for 20 min at 0° C. and 20 min at 25° C. Allyl bromide (0.66 mL, 7.65 mmol) was added. After 5 hr, additional NaH (0.13 g, 3 mmol) and allyl bromide (0.33 mL, 3.5 mmol) were added and stirring was continued for 16 hr. The reaction was quenched with H2O and the solvents removed in vacuo . The residue was partitioned between EtOAc and saturated NaHCO3 solution. The organic layer was separated, washed with brine and dried (MgSO4). Filtration and concentration gave the title compound after chromatography on silica gel with hexane and ethyl acetate 9:1.

1. waitAfter 5 hr
2. stirringstirring
3. waitwas continued for 16 hr
4. customThe reaction was quenched with H2O
5. customthe solvents removed in vacuo
6. customThe residue was partitioned between EtOAc and saturated NaHCO3 solution
7. customThe organic layer was separated
8. washwashed with brine
9. dry with materialdried (MgSO4)
10. filtrationFiltration and concentration