反应详情

温度

70 °C

A 16 mL vial was charged with 3-(benzyloxy)-1-(diphenylmethyl)azetidine (103 mg, 0.31 mmol; which may be prepared as described in Step 1) and 1,2-dichloroethane (1.4 mL). 1-Chloroethyl chloroformate (45 μL, 0.41 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (1.4 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was cooled and concentrated to dryness. The residue was purified on column chromatography (eluent: Pentane/NH3 7N in MeOH, 98/2) to give the title compound (57 mg, 92%).

1. temperatureAfter cooling to room temperature
2. stirringthe reaction mixture was stirred at 70° C. for 1.5 h
3. temperatureThe reaction mixture was cooled
4. concentrationconcentrated to dryness
5. customThe residue was purified on column chromatography (eluent: Pentane/NH3 7N in MeOH, 98/2)