反应详情

A solution of 2-(2-ethoxyphenyl)-8-n-propylpyrido-(3,2-d]pyrimidin-4(3H)-one (Preparation 8; 0.80 g, 0.0026 mol) in a mixture of concentrated sulphuric acid (5.4 ml) and concentrated nitric acid (0.20 ml) was stirred at ambient temperature for 4.5 hours. The mixture was then poured cautiously into stirred ice/water (50 g) and the resulting mixture extracted with a methanol:dichloromethane mixture (1:9, 3×50 ml). The organic extracts were combined, dried (MgSO4) and evaporated under vacuum, and the residue crystallized from ethyl acetate:methanol to give the title compound as an off-white solid (0.71 g, 77%), m.p. 257-259° C.

1. additionThe mixture was then poured cautiously
2. extractionthe resulting mixture extracted with a methanol
3. dry with materialdried (MgSO4)
4. customevaporated under vacuum
5. customthe residue crystallized from ethyl acetate