反应详情

Stir a mixture of 20 g (0.06 mol) 6-(2-fluorophenyl)-5-(4-methoxyphenyl)furo[2,3-d]pyrimidin-4(3H)-one in 78 ml sulpholane and 11 ml (18 g, 0.12 mol) phosphoryl chloride for 1 h at 120° C. After cooling to room temperature, add the reaction solution dropwise to a mixture of 1000 ml water and 100 ml 25% aqueous ammonia solution, stirring vigorously and cooling with ice. Filter off the solid that is precipitated at 10° C. and wash several times with water. Dissolve the solid in 700 ml ethyl acetate again and wash the solution twice with 500 ml water each time. Dry the organic phase over sodium sulphate, filter, and concentrate the filtrate by vacuum evaporation. Mix the residue with 60 ml diisopropyl ether, filter, and dry under vacuum. 18 g (81% of theor.) of the title compound is obtained.

1. additionadd the reaction solution
2. stirringstirring vigorously
3. temperaturecooling with ice
4. filtrationFilter off the solid
5. customthat is precipitated at 10° C.
6. washwash several times with water
7. dissolutionDissolve the solid in 700 ml ethyl acetate again
8. washwash the solution twice with 500 ml water each time
9. dry with materialDry the organic phase over sodium sulphate
10. filtrationfilter
11. concentrationconcentrate the filtrate
12. customby vacuum evaporation
13. additionMix the residue with 60 ml diisopropyl ether
14. filtrationfilter
15. customdry under vacuum