HRID1462117

反应详情

EQUATION

反应方程式

HRID 1462117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

To a mixture of Compound (1) (560 mg.) and N-methylmorpholine (202 mg.) in dichloromethane (30 ml.), there was added isobutyl chloroformate (273 mg.) at -15°~20° C. and the mixture was stirred for 30 minutes at the same temperature. The mixture was cooled to -40° C. and, to this, there was added trimethylsilyl ester of Compound (2), which was prepared from Compound (2) (910 mg.) and bis(trimethylsilyl)acetamide (3 ml.) by stirring in a mixture of dichloromethane (20 ml.) and N,N-dimethylformamide (2 ml.). The mixture was stirred for 1 hour at -15°~-20° C., and then treated in the same manner as the Step 1 of Example 57 to give Compound 3 (1.8 g.).

WORKUP

后处理

  1. stirringThe mixture was stirred for 1 hour at -15°~-20° C.
  2. additiontreated in the same manner as the Step 1 of Example 57