HRID1433596

反应详情

EQUATION

反应方程式

HRID 1433596 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

After adding 2.97 of potassium carbonate and 30 ml of dimethylformamide to 3.09 g of 4-nitrophenol and stirring the mixture at 130° C. for 10 minutes, 2.49 g of 6-(4-benzyloxyphenyl)-4-chloro-7H-pyrrolo[2,3-d]pyrimidine was added and the mixture was further stirred at 130° C. for 5 hours and at 135° C. overnight. After returning the mixture to room temperature, water was added, the precipitated solid was filtered out and subjected to NH silica gel column chromatography (ethyl acetate) and silica gel column chromatography (ethyl acetate), and then ether and ethyl acetate were added prior to sonication. The solid was filtered out to obtain 1.2 g of the title compound.

WORKUP

后处理

  1. stirringthe mixture was further stirred at 130° C. for 5 hours and at 135° C. overnight
  2. customto room temperature
  3. filtrationthe precipitated solid was filtered out
  4. additionether and ethyl acetate were added
  5. customto sonication
  6. filtrationThe solid was filtered out