反应详情

1-Chloroethyl chloroformate (50.0 μL, 0.4 mmol) was added to a solution of 1-benzhydryl-3-(4-methylthiophen-2-ylmethoxy)-azetidine (150.0 mg, 0.4 mmol) in dichloromethane (4.5 mL) at 0° C. The reaction mixture was stirred 3 hours, then 30 minutes at room temperature. Ethanol (6 mL) was added and the reaction mixture was stirred at 35° C. for an additional 4 hours. After concentration to dryness, the crude was triturated in pentane (2×10 mL) to give a yellow solid (94.0 mg, quantitative) which was used in the next step without further purification.

1. custom30 minutes
2. customat room temperature
3. stirringthe reaction mixture was stirred at 35° C. for an additional 4 hours
4. concentrationAfter concentration to dryness
5. customthe crude was triturated in pentane (2×10 mL)
6. customto give a yellow solid (94.0 mg, quantitative) which
7. customwas used in the next step without further purification