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

HRID 598052ノート

反応式

HRID 598052 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-57a353319efd4a0f9f44814c4bb2984f
出典データセット
uspto-grants-2011_03
特許番号
US07897607B2

反応ノート

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