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Hydrogen Peroxide → 3,6-Dichloro-2-[(4-chlorobenzene-1-sulfonyl)(pyridin-4-yl)methyl]pyridine

HRID 748863
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 748863
C(N(CC)CC)C.[S:8](Cl)(Cl)=[O:9].[Cl:12][C:13]1[C:14]([CH:20]([C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)O)=[N:15][C:16]([Cl:19])=[CH:17][CH:18]=1.[Cl:28][C:29]1[CH:34]=[CH:33][C:32](S)=[CH:31][CH:30]=1.C(=O)([O-])[O-:37].[K+].[K+].OO>C(Cl)Cl.C(#N)C.CO.C(OCC)(=O)C.CCCCCC>[Cl:12][C:13]1[C:14]([CH:20]([S:8]([C:32]2[CH:33]=[CH:34][C:29]([Cl:28])=[CH:30][CH:31]=2)(=[O:9])=[O:37])[C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)=[N:15][C:16]([Cl:19])=[CH:17][CH:18]=1
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Komponenten

11

Edukt 6

HCID 784Hydrogen PeroxideHCID 7815p-ChlorothiophenolHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 24386Thionyl ChlorideHCID 23028600(3,6-Dichloropyridin-2-yl) (pyridine-4-yl)methanol

Produkt 1

HCID 23114566
3,6-Dichloro-2-[(4-chlorobenzene-1-sulfonyl)(pyridin-4-yl)methyl]pyridine
Ausbeute 19 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 887MethanolLösungsmittel2×HCID 6342AcetonitrileLösungsmittelHCID 6344DichloromethaneLösungsmittel2×HCID 21226206Ethyl acetate hexaneLösungsmittel

Versuchsvorschrift

Triethylamine (208 μl, 1.89 mmol) and thionyl chloride (138 μl, 1.89 mmol) were added to a solution of (3,6-dichloropyridin-2-yl) (pyridin-4-yl)methanol (161 mg, 0.631 mmol) in methylene chloride (10 ml). After stirring at room temperature for 4 hours, the reaction mixture was concentrated under reduced pressure. Ethyl acetate was added to the residue thus obtained. The resulting mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue thus obtained was dissolved in acetonitrile (10 ml), followed by the addition of 4-chlorobenzenethiol (137 mg, 0.947 mmol) and potassium carbonate (131 mg, 0.947 mmol). Under nitrogen atmosphere, the reaction mixture was stirred at room temperature for 2 days and then at 60° C. for 4 days. The reaction mixture was cooled to room temperature and then, concentrated under reduced pressure. Ethyl acetate was added to the residue thus obtained. The mixture was washed successively with water and brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash chromatography. A fraction obtained from the eluate with 40% ethyl acetate/hexane was concentrated under reduced pressure. The residue thus obtained was dissolved in methanol (10 ml) and to the resulting solution, were added a 30% aqueous hydrogen peroxide solution and hexaammonium heptamolybdate tetrahydrate (73 mg). The reaction mixture was stirred at room temperature for 5 hours. Methanol was distilled off under reduced pressure. A saturated aqueous solution of sodium bicarbonate was added to the concentrated solution thus obtained, followed by extraction with methylene chloride. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash chromatography. A fraction obtained from the eluate with methanol:methylene chloride (=1:80) was concentrated under reduced pressure, whereby the title compound (49 mg, 0.118 mmol, 19%) was obtained as a white solid.

Aufarbeitung

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionEthyl acetate was added to the residue
  3. customthus obtained
  4. washThe resulting mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationAfter filtration
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe residue thus obtained
  9. stirringUnder nitrogen atmosphere, the reaction mixture was stirred at room temperature for 2 days
  10. waitat 60° C. for 4 days
  11. temperatureThe reaction mixture was cooled to room temperature
  12. concentrationconcentrated under reduced pressure
  13. additionEthyl acetate was added to the residue
  14. customthus obtained
  15. washThe mixture was washed successively with water and brine
  16. dry with materialdried over anhydrous sodium sulfate
  17. filtrationfiltered
  18. concentrationThe filtrate was concentrated under reduced pressure
  19. customThe residue thus obtained
  20. concentrationwas concentrated under reduced pressure
  21. customThe residue thus obtained
  22. stirringThe reaction mixture was stirred at room temperature for 5 hours
  23. distillationMethanol was distilled off under reduced pressure
  24. additionA saturated aqueous solution of sodium bicarbonate was added to the concentrated solution
  25. customthus obtained
  26. extractionfollowed by extraction with methylene chloride
  27. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  28. filtrationfiltered
  29. concentrationThe filtrate was concentrated under reduced pressure
  30. customThe residue thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-8754a052bc8549bcb6f292df17776885
Quelldatensatz
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07399775B2

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