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

HRID 979458

반응식

HRID 979458 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 in 300 ml of acetone are heated under reflux for 6 hours. The mixture is then allowed to cool, the solid is filtered off with suction and the mother liquor is evaporated in vacuo. The residue is taken up in methylene chloride, and the solution is washed with water, dried over sodium sulphate and evaporated 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.

후처리

  1. temperatureunder reflux for 6 hours
  2. temperatureto cool
  3. filtrationthe solid is filtered off with suction
  4. customthe mother liquor is evaporated in vacuo
  5. washthe solution is washed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated in vacuo
  8. customThe residue is recrystallised from diethyl ether

출처 및 근거

ORD 기록
ord-b7de8dbd764244a89d31f25d6fa42932
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04668660

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