HRID1689939

反应详情

EQUATION

反应方程式

HRID 1689939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A suspension of 3-(4-bromo-thieno[3,2-d]pyrimidin-2-yl)-phenol (150 mg, 0.49 mmol), 5-tributylstannanyl-thiazole (275 mg, 0.735 mmol), and Pd(PPh3)4 (28 mg, 0.0245 mmol) in anhydrous DMA (4 ml) was heated in a microwave at 150° C. for 15 mins. The reaction was extracted into ethyl acetate, washing with brine and water before drying the organic layer over MgSO4. The crude material was purified by flash column chromatography using 1:1 ethyl acetate/petrol as the eluent. The resulting solid was triturated with dichloromethane to give the title compound as an off-white solid (22 mg, 14%).

WORKUP

后处理

  1. extractionThe reaction was extracted into ethyl acetate
  2. washwashing with brine and water
  3. dry with materialbefore drying the organic layer over MgSO4
  4. customThe crude material was purified by flash column chromatography
  5. customThe resulting solid was triturated with dichloromethane