反应详情

A solution of 5-(5-bromo-2-ethoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one (0.20 g, 0.0051 mol), imidazole (0.172 g, 0.0025 mol), anhydrous potassium carbonate (0.077 g, 0.00056 mol), copper bronze (0.036 g, 0.00057 mol) and iodine (0.015 g, 0.00012 mol) in dimethylformamide (10 ml) was heated under reflux under nitrogen for 4.5 hours, cooled and poured into water (50 ml). This mixture was extracted with a 9:1 mixture of dichloromethane and methanol (6×50 ml) and the extracts combined, dried (MgSO4) and evaporated under vacuum to give a pale brown oil. The oil was chromatographed on silica gel (20 g), eluting with a mixture of dichloromethane, methanol and triethylamine (97.8:20:0.2), to give a yellow solid, crystallisation of which from ethyl acetate-hexane gave the title compound as a cream solid (0.073 g, 38%), m.p. 193°-194° C. Found: C,63.61; H,5.97; N,22.03. C20H22N6O2 requires C,63.48; H,5.86; N,22.21%.

1. temperatureunder reflux under nitrogen for 4.5 hours
2. temperaturecooled
3. extractionThis mixture was extracted with a 9:1 mixture of dichloromethane and methanol (6×50 ml)
4. dry with materialdried (MgSO4)
5. customevaporated under vacuum
6. customto give a pale brown oil
7. customThe oil was chromatographed on silica gel (20 g)
8. washeluting with a mixture of dichloromethane, methanol and triethylamine (97.8:20:0.2)
9. customto give
10. customa yellow solid, crystallisation of which from ethyl acetate-hexane