反应详情

THF (0.8 mL) was added to a reaction vessel containing (S)-tert-butyl 1-(2-methoxyphenyl)-2-oxoazepan-3-ylcarbamate (53 mg, 0.16 mmol). NaH (60% dispersion in oil, 25.4 mg, 0.634 mmol) was then added to the reaction mixture followed by iodomethane (180 mg, 1.27 mmol). The turbid mixture was left to stir at rt for 2 hr. The reaction was quenched by addition of water. The mixture was concentrated to remove some of the THF. The mixture was then partitioned between EtOAc and water. The organic phase was isolated, washed with saturated aqueous NaCl, dried over MgSO4, filtered and concentrated to give (S)-tert-butyl 1-(2-methoxyphenyl)-2-oxoazepan-3-yl(methyl)carbamate (52 mg, 0.15 mmol, 94% yield) as a colorless oil.

1. waitThe turbid mixture was left
2. customThe reaction was quenched by addition of water
3. concentrationThe mixture was concentrated
4. customto remove some of the THF
5. customThe mixture was then partitioned between EtOAc and water
6. customThe organic phase was isolated
7. washwashed with saturated aqueous NaCl
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated