反应详情

温度

50 °C

3-Hydroxyphenylglyoxal (2.10 g, 12.5 mmol) was dissolved in 100 mL of DI water. Acetone oxime (0.912 g, 12.5 mmol) was added, followed by 3 drops of 1N aqueous hydrochloric acid to bring the pH to ca. 2-3. This solution was stirred at 50° C. for one hour, then 2,4,5,6-tetraminopyrimidine sulfate (2.67 g, 11.2 mmol) was added and the reaction mixture was stirred at ambient temperature for 3 hours, then brought to reflux and refluxed for 6 hours. At this point it formed a thick yellow suspension. The reaction was allowed to cool down to ambient temperature. Saturated aqueous sodium bicarbonate was added dropwise to bring the pH to ca. 6-7. The precipitate was collected, washed extensively with water, then with 60 mL of methanol and repeatedly with diethyl ether and dried in vacuo to give 2.75 g of the title compound (96.5% yield) as a light-yellow solid.

1. stirringthe reaction mixture was stirred at ambient temperature for 3 hours
2. temperatureto reflux
3. temperaturerefluxed for 6 hours
4. customAt this point it formed a thick yellow suspension
5. temperatureto cool down to ambient temperature
6. customThe precipitate was collected
7. washwashed extensively with water
8. dry with materialwith 60 mL of methanol and repeatedly with diethyl ether and dried in vacuo