反应详情

To a solution of tert-butyl 2-(1-benzylpiperidin-4-ylcarbamoyl)-6-fluorophenylcarbamate (67.0 g, 157 mmol) in dichloromethane (700 mL) at 0° C. was added trifluoroacetic acid (100 mL). The ice bath was removed and the reaction stirred at room temperature overnight. The reaction was concentrated and partitioned between ethyl acetate and saturated sodium bicarbonate. The aqueous portion was extracted with ethyl acetate (2×), which were washed with water (3×), then brine, dried over magnesium sulfate, and concentrated to give 47.6 g (93%) as a white solid which was used without purification. Mass spec.: 328.33 (MH)+.

1. customThe ice bath was removed
2. concentrationThe reaction was concentrated
3. custompartitioned between ethyl acetate and saturated sodium bicarbonate
4. extractionThe aqueous portion was extracted with ethyl acetate (2×), which
5. washwere washed with water (3×)
6. dry with materialbrine, dried over magnesium sulfate
7. concentrationconcentrated
8. customto give 47.6 g (93%) as a white solid which
9. customwas used without purification