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

HRID 25962

반응식

HRID 25962 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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°.

후처리

  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°)

출처 및 근거

ORD 기록
ord-44df194a82344c0692ea99da4c9c4b5d
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04147793

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