反应详情

温度

70 °C

A 50 mL flask was charged with 1-(diphenylmethyl)-3-(2-thienylmethoxy)azetidine (204 mg, 0.61 mmol; which may be prepared as described in Step 2) and 1,2-dichloroethane (2.7 mL). 1-Chloroethyl chloroformate (86 μL, 0.79 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (2.7 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was concentrated to dryness. The crude mixture was triturated in pentane to give a dark wax (140 mg, quantitative) which was used without further purification.

1. temperatureAfter cooling to room temperature
2. stirringthe reaction mixture was stirred at 70° C. for 1.5 h
3. concentrationThe reaction mixture was concentrated to dryness
4. customThe crude mixture was triturated in pentane
5. customto give a dark wax (140 mg, quantitative) which
6. customwas used without further purification