Benzonitrile, 4-bromo- → 4-Bromo-N-hydroxybenzimidamide

HRID 1003702ノート

反応式

HRID 1003702 の反応式
CC(C)([O-])C.[K+].Cl.[NH2:8][OH:9].[Br:10][C:11]1[CH:18]=[CH:17][C:14]([C:15]#[N:16])=[CH:13][CH:12]=1>CO>[Br:10][C:11]1[CH:18]=[CH:17][C:14]([C:15](=[N:8][OH:9])[NH2:16])=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 12162Benzonitrile, 4-bromo-HCID 443297Hydroxyamine hydrochlorideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 27568384-Bromo-N-hydroxybenzimidamide収率 109.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a stirred solution of ice cooled methanol (115 ml), under argon, was added potassium tert-butoxide (10.12 g. 0.09 mol), portionwise. After stirring for 5 minutes hydroxylamine hydrochloride (6.71 g, 0.097 mol) was added in one portion. After stirring for 1 hour at room temperature a slurry of 4-bromobenzonitrile, (10.88 g, 0.06 mol) in methanol (150 ml) was added. The mixture was then heated at reflux for 4 hours, cooled and filtered. The filtrate was evaporated in vacuo to give the title compound as a colourless solid (14.12 g, quant.)

後処理

  1. additionwas added in one portion
  2. additionwas added
  3. temperatureThe mixture was then heated
  4. temperatureat reflux for 4 hours
  5. temperaturecooled
  6. filtrationfiltered
  7. customThe filtrate was evaporated in vacuo

出典と根拠

ORDレコード
ord-547bb660837142f3bb24e7a104d35fd1
出典データセット
uspto-grants-2000_04
特許番号
US06046210

反応ノート

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