HRID1354293

反应详情

EQUATION

反应方程式

HRID 1354293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(2-Fluoro-phenyl)-3H-thieno[2,3-d]pyrimidin-4-one (900 mg, 3.65 mmole) was dissolved in chloroform and thionyl chloride (0.532 ml, 7.30 mmole) was added to the mixture followed by 1 ml dimethylformamide. Heated the reaction mixture to reflux for 2.5 hours, the cooled mixture was washed with 10% sodium carbonate, dried the chloroform solution over sodium sulfate (anh) and removed solvent. The crude product was chromatographed on silica gel, eluting with chloroform. Upon removal of solvent obtained 438 mg product (yield: 45%).

WORKUP

后处理

  1. temperatureHeated the reaction mixture
  2. temperatureto reflux for 2.5 hours
  3. washthe cooled mixture was washed with 10% sodium carbonate
  4. dry with materialdried the chloroform solution over sodium sulfate (anh)
  5. customremoved solvent
  6. customThe crude product was chromatographed on silica gel
  7. washeluting with chloroform
  8. customUpon removal of solvent