反应详情

Sodium (0.15 g, 0.0013 mol) was added portionwise to ethanol (40 ml) over 1 hour. 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) was then added to the solution and, after 3 days at room temperature, the solvent was removed by evaporation under vacuum. The residual solid was suspended in water (50 ml) and the suspension extracted with ethyl acetate (3×30 ml). The extracts were then combined, dried (Na2SO4) and evaporated under vacuum to give a green solid. Chromatography on silica gel (6 g) using a methanol in dichloromethane elution gradient gave, after crystallisation of the required product from a hexane-ethyl acetate mixture, the title compound as a white solid (0.2 g, 39%) m.p. 89°-90° C. Found C,65,87; H,7.57; N,14.66. C21H28N4O3 requires C,65.60; H,7.34; H,7.34; N,14.57%

1. customthe solvent was removed by evaporation under vacuum
2. extractionthe suspension extracted with ethyl acetate (3×30 ml)
3. dry with materialdried (Na2SO4)
4. customevaporated under vacuum
5. customto give a green solid
6. washa methanol in dichloromethane elution gradient
7. customgave
8. customafter crystallisation of the required product from a hexane-ethyl acetate mixture