碘甲烷 → 5-BROMO-1-METHYL-2(1H)-PYRIDINONE

HRID 40235

反应方程式

HRID 40235 反应方程式
[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:8])[NH:6][CH:7]=1.IC.[C:11](=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:8])[N:6]([CH3:11])[CH:7]=1

参与物

5

反应物 3

HCID 6328碘甲烷HCID 11430碳酸钾HCID 5995282-羟基-5-溴吡啶

产物 1

HCID 130240275-BROMO-1-METHYL-2(1H)-PYRIDINONE

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

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.

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

来源与证据

ORD记录
ord-d95bd4d1ba5843d38255cf8f6ae40564
来源数据集
uspto-grants-2013_09
专利号
US08524900B2

关联笔记

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