反应详情

温度

0 °C

To a cold solution of formic acid (40.2 mL, 1.04 mol) in dichloromethane (150 mL) at 0° C. under a nitrogen atmosphere was added acetic anhydride (15.2 mL, 160 mmol). After 1 h, a solution of 1-(benzyloxyamino-methyl)-cycloheptanecarboxylic acid from Preparation 37 (16.1 mmol theoretical) in dichloromethane (150 mL) was added. The reaction was stirred at 0° C. for 3 h and was concentrated in vacuo. Water (150 mL) was added and the mixture was extracted with dichloromethane (50 mL×5). The combined organic extracts were dried (MgSO4) and were evaporated in vacuo. Purification by preparative, reverse-phase HPLC provided the title compound (2.56 g, 52%). MH+306.

1. additionwas added
2. concentrationwas concentrated in vacuo
3. additionWater (150 mL) was added
4. extractionthe mixture was extracted with dichloromethane (50 mL×5)
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. customwere evaporated in vacuo
7. customPurification by preparative, reverse-phase HPLC