反应详情

7-(3-Methoxyphenyl)-azepan-2-one, as described above in Step C, (0.13 g, 0.6 mmol) and NaH (60% dispersion in mineral oil) (0.03 g, 0.75 mmol) were dissolved in THF (5 mL) under Ar at ambient temperature. After 0.25 hours, iodomethane (0.064 mL, 1.0 mmol) was added and stirring was continued for 20 h. The reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL), the organic layer separated, washed with H2O, dried (MgSO4), filtered and concentrated to give the title compound after SiO2 chromatography (CHCl3:MeOH, 100:1 to 50:1).

1. waitwas continued for 20 h
2. customThe reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL)
3. customthe organic layer separated
4. washwashed with H2O
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated