1H-1,2,4-Triazole → 4-(4-Chlorophenyl)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one

HRID 568314노트

반응식

HRID 568314 반응식
Br[CH2:2][C:3](=[O:15])[C:4]([CH3:14])([CH3:13])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1.[NH:16]1[CH:20]=[N:19][CH:18]=[N:17]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:12][C:9]1[CH:10]=[CH:11][C:6]([CH2:5][C:4]([CH3:14])([CH3:13])[C:3](=[O:15])[CH2:2][N:16]2[CH:20]=[N:19][CH:18]=[N:17]2)=[CH:7][CH:8]=1

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 132865251-Bromo-4-(4-chlorophenyl)-3,3-dimethylbutan-2-one

생성물 1

HCID 132865264-(4-Chlorophenyl)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one수율 356.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

37 g (0.13 mol) of 4-bromo-1-(4-chlorophenyl)-2,2-dimethyl-3-butanone, 13.3 g (0.019 mol) of 1,2,4-triazole and 53.8 g (0.39 mol) of potassium carbonate are heated under reflux in 300 ml of acetone for 8 hours. The mixture is allowed to cool, the inorganic residue is filtered off with suction and the filtrate is concentrated. The residue is taken up in chloroform and the mixture is washed with water, dried over sodium sulphate and concentrated. The residue is stirred with diethyl ether, filtered off with suction and dried at 50° C. in vacuo. 18.8 g (52% of theory) of 1-(4-chlorophenyl)-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-3-butanone of melting point 127° C. are obtained. ##STR18##

후처리

  1. temperatureto cool
  2. filtrationthe inorganic residue is filtered off with suction
  3. concentrationthe filtrate is concentrated
  4. washthe mixture is washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. filtrationfiltered off with suction
  8. customdried at 50° C. in vacuo

출처 및 근거

ORD 기록
ord-2c995d242f9b4e77827f94366a679aff
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728356

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