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

HRID 851128
ノート
印刷プレビュー

反応式

HRID 851128 の反応式
Br[CH:2]([O:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][F:6].[NH:18]1[CH:22]=[N:21][CH:20]=[N:19]1>CC(C)=O>[Cl:17][C:14]1[CH:15]=[CH:16][C:11]([O:10][CH:2]([N:18]2[CH:22]=[N:21][CH:20]=[N:19]2)[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][F:6])=[CH:12][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 92571H-1,2,4-TriazoleHCID 204785111-Bromo-1-(4-chlorophenoxy)-3,3-dimethyl-4-fluoro-2-butanone

生成物 1

HCID 205026601-(4-Chlorophenoxy)-3,3-dimethyl-4-fluoro-1-(1,2,4-triazol-1-yl)-2-butanone収率 89.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

87 g (0.27 mol) of 1-bromo-1-(4-chlorophenoxy)-3,3-dimethyl-4-fluoro-butan-2-one were dissolved in 200 ml of acetone and the solution was added dropwise to a boiling solution of 46 g (0.66 mol) of 1,2,4-triazole in 200 ml of acetone. After heating the mixture under reflux for one hour, the solvent was removed in vacuo, the residue was taken up in methylene chloride, the methylene chloride mixture was washed several times with water and the organic phase was dried over sodium sulphate. After removing the solvent in vacuo, the residue was crystallized with petroleum ether. 75 g (89% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-4-fluoro-1-(1,2,4-triazol-1-yl)-butan-2-one of melting point 60°-63° C. were obtained.

後処理

  1. temperatureAfter heating the mixture
  2. temperatureunder reflux for one hour
  3. customthe solvent was removed in vacuo
  4. washthe methylene chloride mixture was washed several times with water
  5. dry with materialthe organic phase was dried over sodium sulphate
  6. customAfter removing the solvent in vacuo
  7. customthe residue was crystallized with petroleum ether

出典と根拠

ORDレコード
ord-9e43d6cc87bc4e41b4e602888c266046
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04382944

反応ノート

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