反应详情

Allyl bromide (0.02 ml, 0.00023 mol) was added to a stirred suspension of 5-[2-hydroxy-5-(4-methylpiperazinylsulphonyl)-phenyl]-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one (0.103 g, 0.00023 mol) and potassium carbonate (0.032 g, 0.00023 mol) in 2-butanone (10 ml) and the mixture heated under reflux for 8 hours. After cooling, the reaction mixture was evaporated under vacuum and the residue suspended in water (20 ml). The aqueous suspension was extracted with ethyl acetate (3×20 ml), the combined extracts dried (Na2SO4) and, after filtration, evaporated under vacuum to give an oil. Column chromatography on silica gel (2 g) using a methanol in. dichloromethane elution gradient (0-3%), followed by evaporation under vacuum of appropriate fractions, gave a semi-solid which was dissolved in acetone; evaporation under vacuum of the solution gave the title compound (0.011 g, 10%), m.p. 151°-153° C., Rf 0.5 (silica; dichloromethane, methanol; 95:5), m/e 487 (M+ +1).

1. temperaturethe mixture heated
2. temperatureunder reflux for 8 hours
3. temperatureAfter cooling
4. customthe reaction mixture was evaporated under vacuum
5. extractionThe aqueous suspension was extracted with ethyl acetate (3×20 ml)
6. dry with materialthe combined extracts dried (Na2SO4)
7. filtrationafter filtration
8. customevaporated under vacuum
9. customto give an oil
10. washdichloromethane elution gradient (0-3%)
11. customfollowed by evaporation under vacuum of appropriate fractions
12. customgave a semi-solid which
13. customevaporation under vacuum of the solution