Potassium bisulfate → 5-Bromo-1-(difluoromethyl)-1,2-dihydropyridin-2-one

HRID 2245738ノート

反応式

HRID 2245738 の反応式
[Br:1][C:2]1[CH:3]=[CH:4]/[C:5](=N\C(=O)C)/[N:6]([CH:8]([F:10])[F:9])[CH:7]=1.[OH:15]S([O-])(=O)=O.[K+]>CC#N.O>[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:15])[N:6]([CH:8]([F:10])[F:9])[CH:7]=1

参加物

5

反応物 2

HCID 516920Potassium bisulfateHCID 178474078HCID 178474078、化合物

生成物 1

HCID 231159945-Bromo-1-(difluoromethyl)-1,2-dihydropyridin-2-one収率 52%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

To a stirred solution of the crude N-[5-Bromo-1-difluoromethyl-1H-pyridin-(2E)-ylidene]-acetamide (1 g) in 10 ml CH3CN was added 1% KHSO4 in water (10 ml). The reaction mixture was heated at reflux for 3 hrs. The reaction mixture was cooled down and the solvent was removed under reduced pressure. Without any workup this crude was purified by column chromatography using 10% ethyl acetate in hexane to get 5-Bromo-1-difluoromethyl-1H-pyridin-2-one (550 mg, 52%).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 3 hrs
  3. temperatureThe reaction mixture was cooled down
  4. customthe solvent was removed under reduced pressure
  5. customWithout any workup this crude was purified by column chromatography

出典と根拠

ORDレコード
ord-0097fd37b2344a0d97bf4676a40b14de
出典データセット
uspto-grants-2010_03
特許番号
US07683064B2

反応ノート

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