Water → 2-(1,2,4-Triazol-1-yl)-3-phenyl-4'-chlorobutyrophenone

HRID 25962

反応式

HRID 25962 の反応式
[N:1]1([CH2:6][C:7]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1.[H-].[Na+].[CH3:18][CH:19](Cl)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.O>CN(C)C=O>[N:1]1([CH:6]([CH:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH3:18])[C:7]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1

参加物

6

反応物 4

HCID 962WaterHCID 12648(1-Chloroethyl)benzeneHCID 24758Sodium hydrideHCID 7164721-(4-Chlorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethan-1-one

生成物 1

HCID 213260662-(1,2,4-Triazol-1-yl)-3-phenyl-4'-chlorobutyrophenone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-(1,2,4-Triazol-1-yl)-4'-chloroacetophenone (0.01 mol) was dissolved in dimethylformamide (5.0 ml) at room temperature and treated with sodium hydride (0.01 mol). When the reaction was complete (3 hours), the mixture was cooled to 0° and α-methylbenzyl chloride (0.01 mol) was added dropwise with stirring. After stirring at room temperature for 20 hours, the mixture was poured into water and the product filtered off. Recrystallisation from chloroform/petroleum ether (60°-80°) gave the title compound as a colourless crystalline solid, m.p. 163°-5°.

後処理

  1. custom(3 hours)
  2. temperaturethe mixture was cooled to 0°
  3. stirringAfter stirring at room temperature for 20 hours
  4. filtrationthe product filtered off
  5. customRecrystallisation from chloroform/petroleum ether (60°-80°)

出典と根拠

ORDレコード
ord-44df194a82344c0692ea99da4c9c4b5d
出典データセット
uspto-grants-1979_04
特許番号
US04147793

関連ノート

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