HRID1428112

反应详情

EQUATION

反应方程式

HRID 1428112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

HOBt (51 mg), HATU (215 mg), DMAP (23 mg) and DIPEA (131 μl) were added to a solution of the Compound obtained in Step 2 of Example 9 (131 mg) in DMF (2 ml) at room temperature. The reaction mixture was stirred at room temperature for 1.5 hours. The compound obtained in Step 1 of Example 47 (100 mg) was added to the reaction mixture at room temperature. The reaction mixture was stirred at 50° C. for 1.5 hours and returned to room temperature. Water was added to the reaction mixture, and the precipitated solid was collected by filtration. The resulting solid was purified by PLC [dichloromethane:methanol=15:1 (v/v)] to give 64 mg of the title compound as a solid.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at 50° C. for 1.5 hours
  2. customreturned to room temperature
  3. filtrationthe precipitated solid was collected by filtration
  4. customThe resulting solid was purified by PLC [dichloromethane:methanol=15:1 (v/v)]