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

HRID 979458

反応式

HRID 979458 の反応式
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

参加物

5

反応物 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 133403811-Bromo-4-(2,4-dichlorophenyl)-3,3-dimethyl-2-butanone

生成物 1

HCID 133403824-(2,4-Dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone収率 45.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b7de8dbd764244a89d31f25d6fa42932
出典データセット
uspto-grants-1987_05
特許番号
US04668660

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