反应详情

Stir a suspension of 20.0 g (0.06 mol) 5-(4-ethylphenyl)-6-(2-fluorophenyl)furo[2,3-d]pyrimidin-4(3H)-one in 100 ml (165 g, 1.07 mol) phosphoryl chloride for 1 h at 120° C. After cooling to room temperature, add the reaction solution dropwise to a mixture of 330 ml water and 610 ml 25% aqueous ammonia solution, stirring vigorously; a temperature rise to 55-65° C. is observed. Leave the reaction mixture to cool to room temperature. After extracting twice with 500 ml dichloromethane each time, wash the organic phase with satd. aqueous sodium chloride solution, dry over sodium sulphate and filter. Concentrate the filtrate by vacuum evaporation. Mix the residue with 150 ml petroleum ether, filter, wash with ice-cooled petroleum ether and dry under vacuum. 18.7 g (90% purity, 80% of theor.) of the title compound is obtained.

1. additionadd the reaction solution
2. stirringstirring vigorously
3. customto 55-65° C.
4. customLeave the reaction mixture
5. temperatureto cool to room temperature
6. extractionAfter extracting twice with 500 ml dichloromethane each time
7. washwash the organic phase with satd
8. dry with materialaqueous sodium chloride solution, dry over sodium sulphate
9. filtrationfilter
10. concentrationConcentrate the filtrate
11. customby vacuum evaporation
12. additionMix the residue with 150 ml petroleum ether
13. filtrationfilter
14. washwash with ice-
15. temperaturecooled petroleum ether
16. customdry under vacuum