Methyl iodide → 2(1H)-Pyrimidinone, 5-fluoro-1-methyl-

A mixture of the potassium salt of 5-fluoropyrimid-2-one (prepared as described in Undeheim, K. and Gacek, M. Acta. Chem. Scand. 23 (1969) 294 or Budesinsky, Z., Prikyl, J. and Svatek, E. Coll. Czech. Chem. Commun. 30 (1965) 3895) (0.01 mol) and methyl iodide (0.013 mol) in dimethylformamide (40 ml) was stirred at room temperature for 20 hours. The solvent was then removed under reduced pressure (1 mm Hg) and the said residue triturated with chloroform (4×50 ml). The chloroform solution containing the desired product was washed with aqueous 1 N NaOH (3 ml) and with water (3 ml). The dried (MgSO4) chloroform solution was then evaporated and the solid residue recrystallised from benzene; yield 40%, m.p.=177°-178° C. (Found: C, 47.21; H, 3.95; Calc. for C5H5FN2O: C, 46.88; H, 3.93)

1. customThe solvent was then removed under reduced pressure (1 mm Hg)
2. customthe said residue triturated with chloroform (4×50 ml)
3. additionThe chloroform solution containing the desired product
4. washwas washed with aqueous 1 N NaOH (3 ml) and with water (3 ml)
5. dry with materialThe dried (MgSO4) chloroform solution
6. customwas then evaporated
7. customthe solid residue recrystallised from benzene

ORD record

ord-1c43ede1f0c442ba93c6b0caebc2ed96

Source dataset

uspto-grants-1983_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04395406