反应详情

Acetic acid (125 ml) and fuming nitric acid (42.5 ml) were placed in a clean and dry reaction assembly, followed by the addition of 2-propylthio-pyrimidine-4,6-diol (50 g) over a period of 60 minutes at 30-35° C. and with stirring for 1 hour. After completion of the reaction, monitored by TLC, the reaction mass was slowly added to water (250 ml) with maintaining the temperature at below 25° C. The resulting slurry was stirred for 1 hour at 20-25° C. The product was isolated by filtration and washed successively with water (3×100 ml). The wet product was dried under reduced pressure at 40-45° C. to produce 48.28 g of 5-nitro-2-propylthiopyrimidine-4,6-diol as a off-white powder (Purity by HPLC: 99.02 area-%).

1. customdry
2. customreaction assembly
3. customAfter completion of the reaction
4. temperaturewith maintaining the temperature at below 25° C
5. stirringThe resulting slurry was stirred for 1 hour at 20-25° C
6. customThe product was isolated by filtration
7. washwashed successively with water (3×100 ml)
8. customThe wet product was dried under reduced pressure at 40-45° C.