反应详情

A mixture of the product of Example 364B (27.5 g, 0.0618 mol) and pyridine (7.73 g, 7.50 mL, 0.0927 mol, 1.5 equiv.) in dichloromethane (500 mL) was stirred at room temperature. To this mixture was added slowly, dropwise 2,2,2-trichloroethyl chloroformate (17.0 g, 10.8 mL, 0.0803 mol, 1.3 equiv.) over 30 minutes. The reaction mixture was stirred at room temperature for 2 hours, during which time the product precipitated as a yellow solid. The mixture was filtered and the filter cake was rinsed with dichloromethane (100 mL) and dried in vacuo to give the title compound (35.3 g, 92%) as a yellow solid.

1. additionTo this mixture was added slowly
2. stirringThe reaction mixture was stirred at room temperature for 2 hours, during which time the product
3. customprecipitated as a yellow solid
4. filtrationThe mixture was filtered
5. washthe filter cake was rinsed with dichloromethane (100 mL)
6. customdried in vacuo