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1H-1,2,4-Triazole → 3-Methyl-1-(1,2,4-triazol-1-yl)-3-trifluoromethylmercaptobutan-2-one

HRID 1199897
ノート
印刷プレビュー

反応式

HRID 1199897 の反応式
Br[CH2:2][C:3](=[O:12])[C:4]([CH3:11])([S:6][C:7]([F:10])([F:9])[F:8])[CH3:5].[NH:13]1[CH:17]=[N:16][CH:15]=[N:14]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:5][C:4]([S:6][C:7]([F:10])([F:9])[F:8])([CH3:11])[C:3](=[O:12])[CH2:2][N:13]1[CH:17]=[N:16][CH:15]=[N:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 131173011-Bromo-3-methyl-3-trifluoromethylthio-butan-2-one

生成物 1

HCID 130735653-Methyl-1-(1,2,4-triazol-1-yl)-3-trifluoromethylmercaptobutan-2-one収率 62%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

26.5 g (0.1 mol) of 1-bromo-3-methyl-3-trifluoromethylthio-butan-2-one were added dropwise to a mixture of 8.3 g (0.12 mol) of 1,2,4-triazole and 28 g (0.2 mol) of potassium carbonate in 150 ml of acetone at room temperature. The mixture was subsequently stirred under reflux for 1 hour, the inorganic salts were filtered off and the filtrate was concentrated. The residue was taken up in methylene chloride, washed with water, dried over sodium sulphate and distilled. 15.5 g (62% of theory) of 3-methyl-1-(1,2,4-triazol-1-yl)-3-trifluoromethylmercaptobutan-2-one of boiling point 91° C./0.5 mm Hg and of melting point ~45° C. were obtained.

後処理

  1. temperatureunder reflux for 1 hour
  2. filtrationthe inorganic salts were filtered off
  3. concentrationthe filtrate was concentrated
  4. washwashed with water
  5. dry with materialdried over sodium sulphate
  6. distillationdistilled

出典と根拠

ORDレコード
ord-fad554b1996f4af990e6ac88553de98d
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04904297

反応ノート

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