反应详情

温度

110 °C

A mixture of 6-Chloro-9-(2,2-dimethyl-1,3-dioxan-5-ylmethoxy)-2-formamidopurine (630 mg, 1.84 mmol), ammonia (10 ml) and methanol (15 ml) was heated at 110° C. for 7.5 hours in an autoclave and then allowed to cool over 16 hours. The mixture was evaporated to dryness and the residue chromatographed on silica (eluted with chloroform-ethanol, 20:1), affording the title compound (340 mg, 63%). 1R: υmax (KBr) 3409, 3321, 3158, 1669, 1640, 1589, 1488, 1457, 1409 cm-1. H NMR: δH [(CD3)2SO] 1.32(3H,s,CH3), 1.35(3H,s,CH3), 2.00(1H,m,CH3), 3.77(2H,dd, J=11.8, 6.1 Hz, 2×H(ax)), 3.98(2H,dd, J=11.8, 4.1 Hz, 2×H(eq)), 4.32(2H,d, J=7.1 Hz, CH2ON), 5.91(2H,br.s, D2O exchangeable, 6-NH2), 6.78(2H.br,s,D2O exchangeable, 2-NH2), 7.96(1H,s,H-8). Found: C, 48.34; H, 6.18; N, 28.21%; M+ 294.1437. C12H18N6O3 0.2H2O requires: C, 48.37; H, 6.24; N, 28.21%; M+ 294.1440.

1. temperatureto cool over 16 hours
2. customThe mixture was evaporated to dryness
3. customthe residue chromatographed on silica (eluted with chloroform-ethanol, 20:1)