HRID1010824

反应详情

EQUATION

反应方程式

HRID 1010824 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. The reaction mixture was heated to reflux for 2.5 hours, the cooled mixture was washed with 10% sodium carbonate, the chloroform solution was dried over sodium sulfate (anh) and the solvent was removed. The crude product was chromatographed on silica gel, eluting with chloroform. Upon removal of solvent 438 mg of product was obtained (yield: 45%).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 2.5 hours
  3. washthe cooled mixture was washed with 10% sodium carbonate
  4. dry with materialthe chloroform solution was dried over sodium sulfate (anh)
  5. customthe solvent was removed
  6. customThe crude product was chromatographed on silica gel
  7. washeluting with chloroform
  8. customUpon removal of solvent 438 mg of product
  9. customwas obtained (yield: 45%)