反应详情

To a cold solution of formic acid (15.5 mL, 0.40 mol) in dichloromethane (75 mL) at 0° C. under a nitrogen atmosphere was added acetic anhydride (5.9 mL, 62 mmol). After 1 h, a solution of (3S,5R)-1-(Benzyloxyamino-methyl)-3,5-dimethyl-cyclohexanecarboxylic acid (1.8 g, 6.2 mmol) in dichloromethane (75 mL) was added. The reaction was stirred at room temperature for 18 h and was concentrated in vacuo. Water (150 mL) was added and the mixture was extracted with dichloromethane (75 mL×5). The combined organic extracts were dried (MgSO4) and were evaporated in vacuo to yield the title compound as a yellow solid (1.59 g, 80%). MH+320.

1. concentrationwas concentrated in vacuo
2. additionWater (150 mL) was added
3. extractionthe mixture was extracted with dichloromethane (75 mL×5)
4. dry with materialThe combined organic extracts were dried (MgSO4)
5. customwere evaporated in vacuo