反应详情

温度

25 °C

The title compound was prepared as described in WO2010079443A1. To a solution of compound 1-benzhydrylazetidin-3-one (11.7 g, 49.3 mmol) in the methanol (150 mL), tert-butyl hydrazinecarboxylate (6.51 g, 49.3 mmol) was added. Then glacial acetic acid (5.92 mL) was added dropwise at 0° C. The reaction was stirred at 25° C. for 5 h under a nitrogen atmosphere. Then the solvent was evaporated off. The residue was dissolved in dichloromethane (200 mL) and washed with water (2×500 mL). The organic part was dried over sodium sulfate, filtered and concentrated under a vacuum to give the crude tert-butyl 2-(1-benzhydrylazetidin-3-ylidene)hydrazinecarboxylate (16.9 g, 97%) as a white solid. This material was used as is for the next step. MS (ESI, positive ion) m/z (M+1): 352.19.

1. customThen the solvent was evaporated off
2. dissolutionThe residue was dissolved in dichloromethane (200 mL)
3. washwashed with water (2×500 mL)
4. dry with materialThe organic part was dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under a vacuum