HRID507574

反应详情

EQUATION

反应方程式

HRID 507574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2.0 g (15.6 mmol) of 2-thiopheneboronic acid in 80 mL of a 5% (w/v) Na2CO3 aqueous solution was added drop wise to a refluxing solution of 4.7 g (31 mmol) of 2,4-dichloropyrimidine and 0.55 g (0.78 mmol) of bis(triphenylphosphine)palladium(II) chloride in 80 mL of MeCN. The reaction solution was heated at reflux for 6 h, then cooled to rt, the organic solvent removed in vacuo, and the resulting purple solid filtered and washed with water. The crude product was purified by flash chromatography eluting with a linear gradient of neat hexane to neat EtOAc to deliver the title compound. MS (M+H)+ 197.

WORKUP

后处理

  1. temperatureThe reaction solution was heated
  2. temperatureat reflux for 6 h
  3. customthe organic solvent removed in vacuo
  4. filtrationthe resulting purple solid filtered
  5. washwashed with water
  6. customThe crude product was purified by flash chromatography
  7. washeluting with a linear gradient of neat hexane to neat EtOAc