反应详情

温度

80 °C

A suspension of 4.46 g (25 mmol) of diaminodihydroxypyrimidine hydrochloride in 90 ml of toluene and 15.33 g (100 mmol) of phosphorus oxychloride was heated to 80° C. 7.31 g (100 mmol) of dimethylformamide was added drop-wise within a span of 60 minutes. The reaction mixture was then stirred at 80° C. for 16 hours. It was allowed to cool down, and 100 ml of water was then added. The pH was adjusted to 10 using a total of 8.4 g of Na2CO3. The reaction mixture was heated to 40° C. and stirred at this temperature for 4 hours. It was then cooled down to room temperature and neutralized with a 30% solution of NaOH, and the product was filtered off. After washing with water and drying in vacuo, 5.5 g (95%) of product was obtained as a beige solid. This corresponds to a yield of 89%.

1. temperatureto cool down
2. temperatureThe reaction mixture was heated to 40° C.
3. stirringstirred at this temperature for 4 hours
4. temperatureIt was then cooled down to room temperature
5. filtrationthe product was filtered off
6. washAfter washing with water
7. customdrying in vacuo