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

HRID 2165747ノート

反応式

HRID 2165747 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 132865264-(4-Chlorophenyl)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one収率 52%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

37 (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##

後処理

  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

出典と根拠

ORDレコード
ord-b54bfea18e7843d786d98f6c008c0d08
出典データセット
uspto-grants-1990_07
特許番号
US04940798

反応ノート

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