反应详情

A solution of 6-[[1-(t-butyldimethylsilyloxymethyl)-3-(diethoxyphosphoryl)propoxy]amino]-4-chloro-5-formamidopyrimidine (0.5 g) in diethoxymethyl acetate (5 ml) was heated at 110° C. for 2 hours. The solvent was evaporated under reduced pressure, the residue dissolved in methanol (5 ml) and 0.880 ammonia (0.1 ml) added. After 30 minutes at ambient temperature, the solvent was evaporated and the residue chromatographed on silica gel using dichloromethane-methanol (98:2) as eluant. This afforded the title compound (0.27 g, 56%) as a yellow oil. IR: υmax (film) 2940, 2870, 1595, 1565, 1440, 1390, 1340, 1250, 1220, 1060, 1030, 970, 930, 840, 790 cm-1. 1H NMR: δH (CDCl3) 0.0 (6H, s, SiMe2), 0.8 (9H, s, SiBut), 1.25 (6H, t, J=7Hz, (OCH2CH3)2), 1.8-2.4 (4H, m, CH2CH2P) 3.8 (2H, d, J=6Hz, CH2OSi), 4.1 (4H, m, (OCH2CH3)2), 4.6 (1H, m, CHON), 8.35 (1H, s), 8.75 (1H, s). Found: C, 45.97; H, 6.89; N, 10.80%. C19H34N4O5PSiCl requires: C, 46.28; H, 6.95; N, 11.36%.

1. customThe solvent was evaporated under reduced pressure
2. dissolutionthe residue dissolved in methanol (5 ml)
3. addition0.880 ammonia (0.1 ml) added
4. customthe solvent was evaporated
5. customthe residue chromatographed on silica gel