HRID1507877

反应详情

EQUATION

反应方程式

HRID 1507877 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 2-amino-6-(4-fluorophenyl)thieno[2,3-d]pyrimidin-4(3H)-one (50 mg, 0.19 mmol) and BOP (110 mg, 0.25 mmol) in EtOH (1 ml) was added DBU (43 μl, 0.29 mmol). The resulting mixture was heated at 60° C. for 4 hours. After cooling down to room temperature, sodium ethoxide (26 mg, 0.38 mmol) was added. The mixture was again heated at 60° C. overnight. The solvents were removed under reduced pressure and the crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1) yielding the title compound as a white solid (30 mg, 54%).

WORKUP

后处理

  1. temperatureAfter cooling down to room temperature
  2. temperatureThe mixture was again heated at 60° C. overnight
  3. customThe solvents were removed under reduced pressure
  4. customthe crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1)