Methyl iodide → 4-Iodo-1-methylpyridin-2(1H)-one

A solution of 4-iodo-2-pyridone (500 mg), sodium hydride (109 mg) and methyl iodide (482 mg) in dimethylformamide (5.0 mL) was stirred at room temperature for 4 hr. Additional sodium hydride (109 mg) and methyl iodide (482 mg) were added and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with chloroform and washed with saturated aqueous sodium hydrogen carbonate solution. After extraction with chloroform, the organic phase was dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the solvent was then distilled off under reduced pressure. The resulting residue was purified by column chromatography (silica gel cartridge, chloroform:methanol=98:2-96:4) to afford the title compound (341 mg).

1. washwashed with saturated aqueous sodium hydrogen carbonate solution
2. extractionAfter extraction with chloroform
3. dry with materialthe organic phase was dried over anhydrous magnesium sulfate
4. filtrationThe desiccant was filtered off
5. distillationthe solvent was then distilled off under reduced pressure
6. customThe resulting residue was purified by column chromatography (silica gel cartridge, chloroform:methanol=98:2-96:4)

ORD record

ord-9c4b3ac093d64503b4048656d8a7135e

Source dataset

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08729271B2