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

HRID 2198773
ノート
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反応式

HRID 2198773 の反応式
Br[CH:2]([O:10][C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=1[Cl:18])[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][F:6].[NH:19]1[CH:23]=[N:22][CH:21]=[N:20]1>C(#N)C>[Cl:18][C:12]1[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:11]=1[O:10][CH:2]([N:19]1[CH:23]=[N:22][CH:21]=[N:20]1)[C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][F:6]
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 130194441-Bromo-1-(2,4-dichlorophenoxy)-3,3-dimethyl-4-fluoro-2-butanone

生成物 1

HCID 128998841-(2,4-Dichlorophenoxy)-3,3-dimethyl-4-fluoro-1-(1,2,4-triazol-1-yl)-2-butanone収率 89%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

96.3 g (0.27 mol) of 1-bromo-1-(2,4-dichlorophenoxy)-3,3-dimethyl-4-fluoro-2-butanone were dissolved in 200 ml of acetonitrile and the solution was added dropwise to a boiling solution of 46 g (0.56 mol) of 1,2,4-triazole in 200 ml of acetonitrile. After heating the mixture under reflux for 20 hours, 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, 83 g (89% of theory) of 1-(2,4-dichlorophenoxy)-3,3-dimethyl-4-fluoro-1-(1,2,4-triazol-1-yl)-2-butanone were obtained as an oil, which was further reacted directly. ##STR84##

後処理

  1. temperatureAfter heating the mixture
  2. temperatureunder reflux for 20 hours
  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

出典と根拠

ORDレコード
ord-59c9c46fa7724b25be32a56efa0b2e6b
出典データセット
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04359470

反応ノート

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