1H-1,2,4-Triazole → 4-(2,4-Dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone

HRID 329946

반응식

HRID 329946 반응식
Br[CH2:2][C:3](=[O:16])[C:4]([CH3:15])([CH3:14])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:7]=1[Cl:13].[NH:17]1[CH:21]=[N:20][CH:19]=[N:18]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:13][C:7]1[CH:8]=[C:9]([Cl:12])[CH:10]=[CH:11][C:6]=1[CH2:5][C:4]([CH3:15])([CH3:14])[C:3](=[O:16])[CH2:2][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 133403811-Bromo-4-(2,4-dichlorophenyl)-3,3-dimethyl-2-butanone

생성물 1

HCID 133403824-(2,4-Dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone수율 45.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

30 g (0.09 mole) of 1-bromo-4-(2,4-dichlorophenyl)-3,3-dimethyl-2-butanone, 12.4 g (0.18 mole) of 1,2,4-triazole and 24.8 g (0.18 mole) of potassium carbonate are heated under reflux in 300 ml of acetone for 6 hours. The mixture is then allowed to cool and is filtered with suction and the mother liquor is concentrated in vacuo. The residue is taken up in methylene chloride and the mixture is washed with water, dried over sodium sulphate and concentrated in vacuo. The residue is recrystallised from diethyl ether. 12.8 g (45.6% of theory) of 4-(2,4-dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanone of melting point 85° C. are obtained. ##STR14##

후처리

  1. temperatureto cool
  2. filtrationis filtered with suction
  3. concentrationthe mother liquor is concentrated in vacuo
  4. washthe mixture is washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo
  7. customThe residue is recrystallised from diethyl ether

출처 및 근거

ORD 기록
ord-e73acc9589344cf3af29f60ce5376547
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04894382

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