N-bromobutanimide → 3-Bromo-1-methyl-5-nitro-2(1H)-pyridinone

HRID 598052노트

반응식

HRID 598052 반응식
[CH3:1][N:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]1=[O:11].[Br:12]N1C(=O)CCC1=O>CN(C)C=O.ClCCl>[Br:12][C:4]1[C:3](=[O:11])[N:2]([CH3:1])[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=1

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 2958661-methyl-5-nitro-2(1H)-pyridinone

생성물 1

HCID 672674813-Bromo-1-methyl-5-nitro-2(1H)-pyridinone수율 72.15%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

To a solution containing 0.55 g (3.57 mmol) of 1-methyl-5-nitropyridin-2(1H)-one in 10 ml of N,N-dimethylformamide under a nitrogen atm. was added 0.76 g (4.27 mmol) of N-bromosuccinimide. The reaction was allowed to stir at 25° C. overnight. The reaction was diluted with dichloromethane and washed with water. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via biotage eluting with 70% ethyl acetate/hexanes gave 0.60 g (72.15%) of product as a white solid.

후처리

  1. washwashed with water
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. filtrationFiltration, removal of solvent and purification of the residue via biotage
  4. washeluting with 70% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-57a353319efd4a0f9f44814c4bb2984f
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897607B2

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