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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
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HRID 2198773 반응식
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]
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참가 물질

4

반응물 2

HCID 92571H-1,2,4-TriazoleHCID 130194441-Bromo-1-(2,4-dichlorophenoxy)-3,3-dimethyl-4-fluoro-2-butanone

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-59c9c46fa7724b25be32a56efa0b2e6b
출처 데이터셋
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04359470

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