反应详情

温度

100 °C

To a solution of 5-(5-chloromethyl-2-n-propoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one (0.5 g, 0.0013 mol) in dimethyl sulphoxide (10 ml) was added sodium hydroxide (0.26 g, 0.0065 mol) and ethylene glycol (0.41 g, 0.0065 mol). The reaction mixture was heated at 100° C. for 6 hours, allowed to cool and poured into water (50 ml), then the aqueous mixture extracted with ethyl acetate (3>30 ml). The combined extracts were filtered, dried (Na2SO4) and evaporated under vacuum to provide an oil which was purified by chromatography on silica gel (6g), using a methanol in dichloromethane elution gradient (0-3%) methanol). The solid product was crystallised from hexane-ethyl acetate to afford the title compound as a white solid (2%), m.p. 174°-175° C. Found: C,63.97; H,6.66; N,15.57. C19H24N4O3 requires C,64.03; H,6.79; N,15.72%.

1. temperatureto cool
2. extractionthe aqueous mixture extracted with ethyl acetate (3>30 ml)
3. filtrationThe combined extracts were filtered
4. dry with materialdried (Na2SO4)
5. customevaporated under vacuum
6. customto provide an oil which
7. customwas purified by chromatography on silica gel (6g)
8. washa methanol in dichloromethane elution gradient (0-3%) methanol)
9. customThe solid product was crystallised from hexane-ethyl acetate