1H-1,2,4-Triazole → 3,3,4-Trimethyl-1-(1H-1,2,4-triazol-1-yl)pentan-2-one

HRID 1253127ノート

反応式

HRID 1253127 の反応式
Cl[CH2:2][C:3](=[O:10])[C:4]([CH3:9])([CH3:8])[CH:5]([CH3:7])[CH3:6].[NH:11]1[CH:15]=[N:14][CH:13]=[N:12]1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[N:11]1([CH2:2][C:3](=[O:10])[C:4]([CH3:9])([CH3:8])[CH:5]([CH3:7])[CH3:6])[CH:15]=[N:14][CH:13]=[N:12]1

参加物

5

反応物 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 132952261-Chloro-3,3,4-trimethylpentan-2-one

生成物 1

HCID 132952273,3,4-Trimethyl-1-(1H-1,2,4-triazol-1-yl)pentan-2-one収率 79.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

162.5 g (1 mol) of 1-chloro-3,3,4-trimethylpentan-2-one are added dropwise to a suspension of 84 g (1.2 mols) of 1,2,4-triazole and 165.6 g (1.2 mols) of potassium carbonate in 1 liter of ethanol. The mixture is stirred for 15 hours at 40° C., the inorganic precipitate is filtered off under suction, the solvent is distilled off, the precipitate is taken up in 500 ml of methylene chloride, the organic phase is extracted with 1 liter of water, the aqueous phase is extracted with 500 ml of methylene chloride, the methylene chloride phases are combined, and the combined phases are extracted with twice 1 liter of water. The solvent is distilled off from the organic phase. 154.6 g (79.3% of theory) of 1-(1,2,4-triazol-1-yl)-3,3,4-trimethylpentan-2-one are obtained as a colorless oil of refractive index nD20 =1.4827. ##STR16##

後処理

  1. filtrationthe inorganic precipitate is filtered off under suction
  2. distillationthe solvent is distilled off
  3. extractionthe organic phase is extracted with 1 liter of water
  4. extractionthe aqueous phase is extracted with 500 ml of methylene chloride
  5. extractionthe combined phases are extracted with twice 1 liter of water
  6. distillationThe solvent is distilled off from the organic phase

出典と根拠

ORDレコード
ord-19dde3c20ea545b2aa8ff9e78b990536
出典データセット
uspto-grants-1988_05
特許番号
US04747869

反応ノート

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