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

5-Bromopyridin-2(1H)-one (0.250 g, 1.44 mmol) was dissolved in DMF (3 mL) then added iodomethane (0.0943 ml, 1.51 mmol) and potassium carbonate (0.218 g, 1.58 mmol). The reaction was stirred at room temperature overnight. The reaction mixture was concentrated under vacuum. The remaining residue was dissolved in ethyl acetate then washed with water and brine. The aqueous layer was back-extracted with ethyl acetate (3×). The organic layers were combined and dried over sodium sulfate then concentrated under vacuum to afford 5-bromo-1-methylpyridin-2(1H)-one as an orange waxy solid.

1. concentrationThe reaction mixture was concentrated under vacuum
2. dissolutionThe remaining residue was dissolved in ethyl acetate
3. washthen washed with water and brine
4. extractionThe aqueous layer was back-extracted with ethyl acetate (3×)
5. dry with materialdried over sodium sulfate
6. concentrationthen concentrated under vacuum

ORDレコード

ord-d95bd4d1ba5843d38255cf8f6ae40564

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08524900B2