反应详情

A mixture of pyrido[2,3-d]pyrimidin-4(3H)-one (1.471 g, 10 mM) and POCl3 (16 ml) is stirred for 1 h at reflux. The excess of POCl3 is removed under vacuum. Then dichloromethane and iced water is added and the mixture stirred until the black solid dissolves. The organic layer is separated, washed with bicarbonate solution, dried over Na2SO4 and then evaporated to dryness. The yellow residue is recrystallized from toluene/hexane to give almost pure title compound in 70% yield. mp 137° C.

1. temperatureat reflux
2. customThe excess of POCl3 is removed under vacuum
3. additionThen dichloromethane and iced water is added
4. stirringthe mixture stirred until the black solid
5. dissolutiondissolves
6. customThe organic layer is separated
7. washwashed with bicarbonate solution
8. dry with materialdried over Na2SO4
9. customevaporated to dryness
10. customThe yellow residue is recrystallized from toluene/hexane