反应详情

4-Amino-2-chloro-6,7-dimethoxyquinazoline (0.8 g, 3.3 mmole) and 2-phenoxy-4-piperazinopyrimidine dihydrochloride (1.2 g, 3.6 mmole) were heated under reflux in n-butanol (50 ml) overnight. The mixture was then evaporated in vacuo and the residue partitioned between chloroform/methanol/saturated aqueous sodium carbonate solution (300 ml:100 ml:50 ml). The chloroform/methanol layer was separated, dried (Na2SO4), evaporated in vacuo then the residue (1 g) chromatographed on silica gel (85 g). The column was eluted with chloroform, then chloroform containing 2.5% methanol by volume, appropriate fractions combined, evaporated in vacuo and the residue recrystallized from ethanol to give the title compound, (0.14 g) m.p. 253°-254° C.

1. customThe mixture was then evaporated in vacuo
2. customthe residue partitioned between chloroform/methanol/saturated aqueous sodium carbonate solution (300 ml:100 ml:50 ml)
3. customThe chloroform/methanol layer was separated
4. dry with materialdried (Na2SO4)
5. customevaporated in vacuo
6. customthe residue (1 g) chromatographed on silica gel (85 g)
7. washThe column was eluted with chloroform
8. customevaporated in vacuo
9. customthe residue recrystallized from ethanol