反应详情

温度

160 °C

P2O5 (0.29 g) and H3PO4 (0.21 mL) were added to a mixture of N-(4,6-diaminopyrimidin-5-yl)-4-phenyl-1-{[2- trimethylsilyl)ethoxy]methyl}-1H-imidazole-5-carboxamide and N-(4,6-diaminopyrimidin-5-yl)-5-phenyl-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazole-4-carboxamide (Intermediate 36) (65 mg) and heated at 160° C. for 24 hours. After cooling to ambient temperature, ice was added and the reaction mixture adjusted to pH 5 with NH3 solution. The solvent was evaporated in vacuo to give a yellow oil. Purification by preparative RPHPLC (MeCN:water:TFA, 90:10:0.1) gave the title compound as a colourless solid (2.6 mg, 6%);

1. temperatureAfter cooling to ambient temperature
2. additionice was added
3. customThe solvent was evaporated in vacuo
4. customto give a yellow oil
5. customPurification by preparative RPHPLC (MeCN:water:TFA, 90:10:0.1)