反应详情

Ethyl [(4,6-dimethoxypyrimidin-2-yl)amino carbonothioylcarbamate (0.50 g, 1.7 mmol) was mixed with ethanol (5 mL). To this mixture was added hydroxylamine hydrochloride (0.12 g, 1.7 mmol) and diisopropylethyl-amine (0.30 mL, 1.7 mmol). The resulting mixture was allowed to stir at room temperature. After 2.5 hours, additional diisopropylethylamine (0.30 mL, 1.7 mmol) was added to the mixture. After 48 hours the ethanol was removed in vacuo and the residue was partitioned between H2O and Et2O to give a powder. The powder was filtered and dried to afford the product as a tan powder (0.27 g, 82%). mp 215-220° C. Anal: Cacld for C7H9N5O2: C, 43.08; H, 4.65; N, 35.88; O, 16.39; found: C, 39.88; H, 4.22; N, 32.00; O, 16.35. 1H NMR (DMSO-d6): δ 6.04 (s, 1H); 5.97 (br, 2H); 4.04 (s, 3H).

1. customAfter 48 hours the ethanol was removed in vacuo
2. customthe residue was partitioned between H2O and Et2O
3. customto give a powder
4. filtrationThe powder was filtered
5. customdried