Methyl iodide → 5-Bromo-1-methylpyridin-2(1H)-one

Participants

Reaction Conditions

Reaction Steps

The mixture of 5-bromo-2(1H)-pyridone (200 g) and MeI (324 g) and K2CO3 (318 g) in DME (2 l) was heated at 80° C. with stirring for 2 hours. The above mixture was cooled to room temperature. The precipitated salt was removed by filtration and washed with DME. Evaporation of solvent in the filtrate in vacuo gave oily residue. The residue was portioned to EtOAc and water. The organic layer was separated. Aqueous layer was extracted with EtOAc twice. The combined organic solution was dried over MgSO4. Evaporation of solvent in vacuo gave crystal residue. The residue was pulverized with IPE and n-hexane (1:3, 1000 ml). The precipitate was collected by filtration and dried in vacuo to give 5-bromo-1-methyl-2(1H)-pyridone as white powder (182.5 g).

Provenance & Evidence