Acetonitrile → 1-Phenyl-2-(1H-1,2,4-triazol-1-yl)propan-1-one

HRID 483116ノート

反応式

HRID 483116 の反応式
Br[CH:2]([CH3:11])[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].N1C=[CH:15][N:14]=[N:13]1.[C:17](#[N:19])C>>[N:14]1([CH:2]([CH3:11])[C:3]([C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)=[O:4])[CH:15]=[N:19][CH:17]=[N:13]1

参加物

4

反応物 3

HCID 6342Acetonitrile2 回HCID 164522-BromopropiophenoneHCID 178418936HCID 178418936、化合物

生成物 1

HCID 132599821-Phenyl-2-(1H-1,2,4-triazol-1-yl)propan-1-one収率 55%

実験手順

To a solution of 223 g (1 mol) of 2-bromopropiophenone in 300 ml of acetonitrile is added dropwise to a boiling mixture of 414 g (6 mols) of triazole and 1,200 ml of acetonitrile, and the mixture is heated at the boil for 8 hours. Thereafter, the mixture is evaporated down in vacuo, the residue is taken up in 750 ml of dichloromethane and 750 ml of water, and the organic phase is washed with several 500 ml portions of water and dried over anhydrous sodium sulphate. After the solvent has been distilled off, the remaining residue is distilled in vacuo. 111 g (55% of theory) of 2-(1,2,4-triazol-1-yl)-propiophenone of boiling point 133° C./0.15 mbar and of melting point 117° C. are obtained. ##STR21##

後処理

  1. temperaturethe mixture is heated at the boil for 8 hours
  2. customThereafter, the mixture is evaporated down in vacuo
  3. wash750 ml of water, and the organic phase is washed with several 500 ml portions of water
  4. dry with materialdried over anhydrous sodium sulphate
  5. distillationAfter the solvent has been distilled off
  6. distillationthe remaining residue is distilled in vacuo

出典と根拠

ORDレコード
ord-4f62a252fa864e88abf63685df811bea
出典データセット
uspto-grants-1986_03
特許番号
US04578396

反応ノート

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