HRID2181353

反应详情

EQUATION

反应方程式

HRID 2181353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

5-Bromo-3-methyl-1-(2-methylpropyl)-6-[[2-(trifluoromethyl)phenyl]methyl]-thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione, (0.35 g, Example 1c)), thiophene-3-boronic acid (0.053 g), barium hydroxide octahydrate (0.15 g) and tetrakis(triphenylphosphine)palladium (0) (0.0097 g) in ethylene glycol dimethyl ether (6 ml) and water (1 ml) were combined in a sealed vial and stirred with heating at 80° C. for 18 hours. After cooling, the reaction mixture was absorbed onto silica and purified by flash silica chromatography eluting with 25% ethyl acetate in isohexane to give an oil. The oil was triturated with isohexane, filtered and dried under vacuum to give the title compound as a beige solid (0.020 g).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe reaction mixture was absorbed onto silica
  3. custompurified by flash silica chromatography
  4. washeluting with 25% ethyl acetate in isohexane
  5. customto give an oil
  6. customThe oil was triturated with isohexane
  7. filtrationfiltered
  8. customdried under vacuum