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

HRID 434378

反応式

HRID 434378 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d8c15482729c4ec7a030997491fe14e4
出典データセット
uspto-grants-1983_08
特許番号
US04396624

関連ノート

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