反应详情

温度

90 °C

A suspension of 1-methyl-2,3-dihydroimidazo[1,2-c]pyrimidine-5,7(1H,6H)-dione (0.41 g, 2.45 mmol) in POCl3 (15 mL, 161 mmol) was stirred at 90° C. for 6 h. The suspension was concentrated in vacuo to remove all of POCl3. Cold water was added to the resultant residue, and then solid NaOH was added dropwise to adjust pH to ˜12. The solution was stirred at rt for 2 h. Aqueous HCl was added to adjust pH to ˜7. Purification via Mass Directed AutoPrep (MDAP) afforded the title compound as a white solid (0.42 g, 93% yield).

1. concentrationThe suspension was concentrated in vacuo
2. customto remove all of POCl3
3. additionCold water was added to the resultant residue
4. additionsolid NaOH was added dropwise
5. stirringThe solution was stirred at rt for 2 h
6. additionAqueous HCl was added
7. customPurification via Mass Directed AutoPrep (MDAP)