Ammonia → HCID 19808601, compound

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A solution of 4-chloro-6-[[3-(diethoxyphosphoryl)-propoxy]amino]-5-formamidopyrimidine (0.86 g, 2.3 mmol) in diethoxymethyl acetate (5 ml) was heated at 120° C. for 2 hours. After cooling to ambient temperature, excess solvent was removed under reduced pressure to leave an oil. The oil was dissolved in methanol (20 ml) and 880 ammonia (0.5 ml) was added. After 20 minutes at ambient temperature, the solvent was evaporated to leave an oil. Purification by column chromatography on silica gel (dichloromethane:methanol, 96:4 as eluant) gave the title compound as a yellow oil (0.7 g, 85%). IR: υmax 3065, 3000, 1595, 1560, 1330, 1240, 1215, 1160, 1050, 1025, 960 and 930 cm-1. 1H NMR: δH [(CD3)2SO] 1.22 (6H, t, J=7Hz, (OCH2CH3)2), 1.6-2.1 (4H, m, OCH2CH2CH2P), 4.00 (4H, m, (OCH2CH3)2), 4.50 (2H, t, J=6Hz, OCH2), 8.8 (1H, s), 9.05 (1H, s).

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