反应详情

Methanesulphonyl chloride (0.157 g, 0.00137 mol) was added to a stirred solution of 5-(5-amino-2-ethoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one (0.45 g, 0.00137 mol) in dry pyridine (30 ml) at 0° C. The mixture was stirred for 18 hours at room temperature and then evaporated under vacuum. The residue was suspended in saturated aqueous sodium bicarbonate solution (50 ml) and the mixture extracted with dichloromethane (2×30 ml). The organic extracts were combined, washed with brine (2×30 ml), dried (Na2SO4) an evaporated under vacuum. The residue was triturated with ether, chromatographed on silica gel (12 g), eluting with a 98.5:1.5 mixture of dichloromethane and methanol, and the required product crystallised form ethyl acetate-hexane to give the title compound as a white powder (0.32 g, 58%), m.p. 205°-206° C. Found: C,53.63; H,5.66; N,17.24. C18H23N5O4S requires C,53.32; H,5.72; N,17.27%.

1. customevaporated under vacuum
2. extractionthe mixture extracted with dichloromethane (2×30 ml)
3. washwashed with brine (2×30 ml)
4. dry with materialdried (Na2SO4)
5. customan evaporated under vacuum
6. customThe residue was triturated with ether
7. customchromatographed on silica gel (12 g)
8. washeluting with a 98.5:1.5 mixture of dichloromethane and methanol
9. customthe required product crystallised
10. customform ethyl acetate-hexane