反应详情

温度

130 °C

To a mixture of 6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4(3H)-one (30.0 g) and toluene (240 mL) were added phosphorous oxychloride (40 mL) and DMF (1.0 mL), followed by heating to reflux at 130° C. for 2 hours. The reaction mixture was left to be cooled to room temperature and concentrated under reduced pressure. To the residue were added chloroform and saturated aqueous sodium bicarbonate, followed by stirring. The organic layer was washed sequentially with water and brine. To the organic layer were added MgSO4, activated carbon (10 g), and silica gel (100 mL), followed by stirring. The mixture was filtered through Celite and then concentrated under reduced pressure to obtain 4-chloro-6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidine (31.3 g).

1. temperatureby heating
2. waitThe reaction mixture was left
3. temperatureto be cooled to room temperature
4. concentrationconcentrated under reduced pressure
5. additionTo the residue were added chloroform and saturated aqueous sodium bicarbonate
6. washThe organic layer was washed sequentially with water and brine
7. additionTo the organic layer were added MgSO4, activated carbon (10 g), and silica gel (100 mL)
8. stirringby stirring
9. filtrationThe mixture was filtered through Celite
10. concentrationconcentrated under reduced pressure