反应详情

To a solution of 1-benzyloxycarbonylamino-cyclopropanecarboxylic acid (7.0 g, 29.8 mmol) in DMF (30 mL) was added HATU (11.3 g, 29.8 mmol) and Et3N (4.3 mL, 29.8 mmol). The mixture was allowed to stir at room temperature for 20 min, then ammonium hydrogen carbonate (7.06 g, 89.3 mmol) was added in one portion. The reaction was heated at 60° C. for 12 h. The mixture was cooled to room temperature, diluted with water and extracted with EtOAc (2×100 mL). The combined extracts were washed with satd NaHCO3, water, brine and dried with MgSO4. The mixture was filtered and the solvent removed to give (1-carbamoyl-cyclopropyl)-carbamic acid benzyl ester (5.5 g, 24.5 mmol) as a white solid.

1. temperatureThe reaction was heated at 60° C. for 12 h
2. temperatureThe mixture was cooled to room temperature
3. extractionextracted with EtOAc (2×100 mL)
4. washThe combined extracts were washed with satd NaHCO3, water, brine
5. dry with materialdried with MgSO4
6. filtrationThe mixture was filtered
7. customthe solvent removed