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

HRID 434378

반응식

HRID 434378 반응식
Cl[CH2:2][C:3](=[O:8])[C:4]([CH3:7])([CH3:6])[CH3:5].[NH:9]1[CH:13]=[N:12][CH:11]=[N:10]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:5][C:4]([CH3:7])([CH3:6])[C:3](=[O:8])[CH2:2][N:9]1[CH:13]=[N:12][CH:11]=[N:10]1

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 835721-Chloropinacolone

생성물 1

HCID 1008773,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone수율 74%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

13.45 g (1 mol) of 1-chloro-3,3-dimethyl-butan-2-one, 69 g (1 mol) of 1,2,4-triazole and 140 g (1 mol) of powdered potassium carbonate were heated under reflux in 500 ml of acetone for 6 hours, while stirring. Thereafter, the mixture was allowed to cool, the inorganic salt was filtered off and the filtrate was concentrated in vacuo. After treatment with diisopropyl ether, the oily residue crystallized out. After drying, 123.6 g (74% of theory) of 3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one of melting point 63°-65° C. were obtained.

후처리

  1. temperatureto cool
  2. filtrationthe inorganic salt was filtered off
  3. concentrationthe filtrate was concentrated in vacuo
  4. customAfter treatment with diisopropyl ether, the oily residue crystallized out
  5. customAfter drying

출처 및 근거

ORD 기록
ord-d8c15482729c4ec7a030997491fe14e4
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04396624

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