Sodium Acetate → 6-ethyl-5-fluoro-4(3H)-pyrimidone

To the product of part (iv) (6 g) in ethanol (60 ml) was added sodium acetate (5.5 g) and 5% palladium-on-carbon (0.6 g). The mixture was hydrogenated at 3 atmospheres pressure for 8 hours. The catalyst was removed by filtration and the filtrate was concentrated to a volume of 10 ml then mixed with water (2 ml) and dichloromethane (80 ml). Toluene (32 ml) was added and the solution was concentrated to a volume of 5-6 ml and then mixed with further toluene (8 ml). The crystals of the title compound that separated were isolated by filtration and characterised by 1 H-NMR and mass spectrometry (Yield=3.9 g).

1. customThe catalyst was removed by filtration
2. concentrationthe filtrate was concentrated to a volume of 10 ml
3. additionthen mixed with water (2 ml) and dichloromethane (80 ml)
4. additionToluene (32 ml) was added
5. concentrationthe solution was concentrated to a volume of 5-6 ml
6. additionmixed with further toluene (8 ml)
7. customThe crystals of the title compound that separated
8. customwere isolated by filtration

ORD record

ord-03ad7e56a315404aafdbe7bd50f162ab

Source dataset

uspto-grants-1998_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05773443