HRID40235

反应详情

EQUATION

反应方程式

HRID 40235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  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