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Hydrogen Peroxide → 3-Fluoro-2-phenylsulfinyl-5-trifluoromethylpyridine

HRID 636067
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HRID 636067 반응식
[F:1][C:2]1[C:3]([S:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.FC(F)(F)C(O)=[O:22].OO>C(O)(=O)C>[F:1][C:2]1[C:3]([S:12]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)=[O:22])=[N:4][CH:5]=[C:6]([C:8]([F:9])([F:10])[F:11])[CH:7]=1
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참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 6422Trifluoroacetic acidHCID 184665183-Fluoro-2-phenylthio-5-trifluoromethylpyridine

생성물 1

HCID 184665193-Fluoro-2-phenylsulfinyl-5-trifluoromethylpyridine

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
22 °C

실험 절차

20 g (0.0693 mol) of 95% pure 3-fluoro-2-phenylthio-5-trifluoromethylpyridine were introduced into 100 ml of glacial acetic acid and 20 ml of trifluoroacetic acid and over a period of 5 min, with stirring at 22° C., 5.64 g (0.083 mol) of 50% strength hydrogen peroxide were added. The reaction mixture was stirred at 22° C. for 10 h and then poured into 1 l of ice-water and extracted with methylene chloride. The organic phase was washed with saturated sodium bicarbonate solution and water. After drying, filtration through silica gel and concentration under reduced pressure, 19.1 g (95.4% of theory) of the title compound of 24 n D

후처리

  1. stirringThe reaction mixture was stirred at 22° C. for 10 h
  2. extractionextracted with methylene chloride
  3. washThe organic phase was washed with saturated sodium bicarbonate solution and water
  4. customAfter drying
  5. filtrationfiltration
  6. concentrationthrough silica gel and concentration under reduced pressure, 19.1 g (95.4% of theory) of the title compound of 24 n D

출처 및 근거

ORD 기록
ord-b9b1d0163ddc4a40b4e2f3efd531e50b
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06191280B1

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