Uracil → 5-Nitrosouracil

Temperatur

10 °C

1-Propyl, 3-cyclopropyl, 6-aminouracil (2) (12.8 g, 61.2 mmol ) was dissolved in acetic acid (25 ml) in 200 ml of water and the mixture was cooled to 10° C. To the uracil solution, NaNO2 (7.6 g, 110.1 mmol ) in 50 ml of water was added dropwise at 10° C. The mixture was stirred at 10° C. for 30 min and then at room temperature for 1 h. The solvent was removed under reduced pressure and the residue was dissolved in the mixture of absolute ethanol and CH2Cl2 (1:1) and boiled for 20 min. The hot mixture was filtered through a layer of Celite 545 to remove the insoluble inorganic salts. The mother liquid was evaporated under reduced pressured to remove the solvent to give 1-propyl, 3-cyclopropyl, 6-amino, 5-nitrosouracil (4) (11.4 g, 78%).

1. waitat room temperature for 1 h
2. customThe solvent was removed under reduced pressure
3. dissolutionthe residue was dissolved in the mixture of absolute ethanol and CH2Cl2 (1:1)
4. waitboiled for 20 min
5. filtrationThe hot mixture was filtered through a layer of Celite 545
6. customto remove the insoluble inorganic salts
7. customThe mother liquid was evaporated
8. customto remove the solvent

ORD-Eintrag

ord-211ed4aa03e1415586630c87f5b4b3d4

Quelldatensatz

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07598379B2