HRID1354293
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureHeated the reaction mixture
- temperatureto reflux for 2.5 hours
- washthe cooled mixture was washed with 10% sodium carbonate
- dry with materialdried the chloroform solution over sodium sulfate (anh)
- customremoved solvent
- customThe crude product was chromatographed on silica gel
- washeluting with chloroform
- customUpon removal of solvent