Nitric Acid → HCID 178460811, compound

Temperature

27.5 °C

To a clean and dry reaction assembly containing acetic acid (1000 ml) was added fuming nitric acid (340 ml) over a period of 15 to 20 minutes, while maintaining the temperature between 25-30° C. 2-Propylthio-pyrimidine-4,6-diol (400 g) was added to the mixture over a period of 60 minutes at 25-30° C., followed by rinsing of flask with acetic acid (100 ml). The resulting mass was stirred for 1 hour at 25-30° C. After completion of the reaction, water (2400 ml) was added to the mass for 20 minutes at 25-30° C. The resulting slurry was stirred for 1 hour at 25-30° C. The product was isolated by filtration and washed successively with water (4×800 ml). The wet product was dried under reduced pressure at 50-55° C. to produce the 5-nitro-2-propylthiopyrimidine-4,6-diol as a off-white to yellow powder (375 g, HPLC purity: 99.06% by area).

1. customTo a clean and dry
2. customreaction assembly containing acetic acid (1000 ml)
3. washby rinsing of flask with acetic acid (100 ml)
4. customAfter completion of the reaction, water (2400 ml)
5. additionwas added to the mass for 20 minutes at 25-30° C
6. stirringThe resulting slurry was stirred for 1 hour at 25-30° C
7. customThe product was isolated by filtration
8. washwashed successively with water (4×800 ml)
9. customThe wet product was dried under reduced pressure at 50-55° C.

ORD record

ord-09c017fabb154758b12e63ce322da674

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08859769B2