Dimethylformamide → 1-(2-Pyridyl)-5-(2-pyridyl)-3-bromo-1,2-dihydropyridin-2-one

HRID 229642노트

반응식

HRID 229642 반응식
CN(C)C=O.[N:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N:12]1[CH:17]=[C:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[CH:15]=[CH:14][C:13]1=[O:24].[Br:25]N1C(=O)CCC1=O>O>[N:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N:12]1[CH:17]=[C:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[CH:15]=[C:14]([Br:25])[C:13]1=[O:24]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 67184N-bromobutanimideHCID 223189481-(2-Pyridyl)-5-(2-pyridyl)-1,2-dihydropyridin-2-one

생성물 1

HCID 223190411-(2-Pyridyl)-5-(2-pyridyl)-3-bromo-1,2-dihydropyridin-2-one수율 54.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2 ml of a dimethylformamide solution containing 0.07 g of 1-(2-pyridyl)-5-(2-pyridyl)-1,2-dihydropyridin-2-one was incorporated with 0.07 g of N-bromosuccinic acid imide, under stirring and ice-cooling. After stirring the mixture at room temperature for 2 hours, it was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and brine, and then dried over magnesium sulfate. The solvent was evaporated, and the residue was purified by silica gel chromatography (ethyl acetate/hexane=3:1), to give 0.05 g of the title compound as a pale brown powder.

후처리

  1. temperatureice-cooling
  2. stirringAfter stirring the mixture at room temperature for 2 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated
  7. customthe residue was purified by silica gel chromatography (ethyl acetate/hexane=3:1)

출처 및 근거

ORD 기록
ord-097aadcdb5cb48f2b852bc58476ec410
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563811B2

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