反应详情

Trifluoroacetic acid (60 mL) was added to a solution of benzyl (3R)-6-(2,3-difluorophenyl)-1-(2,4-dimethoxybenzyl)-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-ylcarbamate (3.70 g, 7.08 mmol) in dichloromethane (40 mL). After 18 h, the mixture was concentrated at 25° C., methanol (150 mL) was added, and the precipitate filtered. The filtrate was concentrated, diluted with dichloromethane (100 mL), washed with water (2×), saturated aqueous sodium bicarbonate (2×), saturated brine, dried over magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography (5% ethyl acetate/hexanes→65% ethyl acetate/hexanes) gave the title compound (1.75 g). MS 373.1 (M+1).

1. concentrationthe mixture was concentrated at 25° C.
2. additionmethanol (150 mL) was added
3. filtrationthe precipitate filtered
4. concentrationThe filtrate was concentrated
5. additiondiluted with dichloromethane (100 mL)
6. washwashed with water (2×), saturated aqueous sodium bicarbonate (2×), saturated brine
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated
10. customPurification by silica gel chromatography (5% ethyl acetate/hexanes→65% ethyl acetate/hexanes)