反应详情

A mixture of thieno[2,3-d]pyrimidin-4-ol derivative 3 (3.7 mmol), thionyl chloride (5.5 mL) and dry DMF (0.5 mL) was heated at reflux for 4 h. The reaction mixture was cooled to room temperature and the excess thionyl chloride was removed by vacuum distillation. To the resulting residue 200 g of ice was added and extracted with dichloromethane (3×100 mL). The combined organic layers were dried (Na2SO4) and concentrated. The product was purified by silica chromatography (100% DCM) to afford 4-Chloro-thieno[2,3-d]-pyrimidine 4 in 80-95% yields.

1. temperaturewas heated
2. temperatureat reflux for 4 h
3. customthe excess thionyl chloride was removed by vacuum distillation
4. additionTo the resulting residue 200 g of ice was added
5. extractionextracted with dichloromethane (3×100 mL)
6. dry with materialThe combined organic layers were dried (Na2SO4)
7. concentrationconcentrated
8. customThe product was purified by silica chromatography (100% DCM)