Methyl iodide → 5-Bromo-1-methyl-3-nitropyridin-2(1H)-one

HRID 1671605노트

반응식

HRID 1671605 반응식
[C:1](=[O:4])([O-])[O-].[Cs+].[Cs+].[Br:7][C:8]1[CH:9]=[C:10]([N+:15]([O-:17])=[O:16])[C:11](O)=[N:12][CH:13]=1.IC>CN(C)C=O>[Br:7][C:8]1[CH:9]=[C:10]([N+:15]([O-:17])=[O:16])[C:1](=[O:4])[N:12]([CH3:11])[CH:13]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 178418997HCID 178418997, 화합물

생성물 1

HCID 529112535-Bromo-1-methyl-3-nitropyridin-2(1H)-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Cesium carbonate (44.6 g, 137 mmol) was added to a solution of 5-bromo-2-hydroxy-3-nitropyridine (20.0 g, 91.3 mmol) and iodomethane (19.4 g, 137 mmol) in N,N-dimethylformamide (500 mL). After 18 h, the reaction mixture was quenched with water. The mixture was extracted with ethyl acetate (3×), and the combined organic extracts were washed with water, saturated brine, dried over sodium sulfate, filtered and concentrated. MS 233.1 (MI).

후처리

  1. customthe reaction mixture was quenched with water
  2. extractionThe mixture was extracted with ethyl acetate (3×)
  3. washthe combined organic extracts were washed with water, saturated brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-189957b88567458ca99b66bcd6f68641
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994325B2

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