Methanesulfenyl chloride, trifluoro- → HCID 22591644, Verbindung

HRID 22866Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 22866
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:17]([NH:18][CH2:19][C:20]2[CH:25]=[N:24][CH:23]=[CH:22][N:21]=2)=[CH:16][CH:15]=[N:14]1.[F:26][C:27]([F:31])([F:30])[S:28]Cl.C(=O)([O-])O.[Na+]>C(Cl)Cl>[Cl:12][C:4]1[CH:5]=[C:6]([C:8]([F:9])([F:10])[F:11])[CH:7]=[C:2]([Cl:1])[C:3]=1[N:13]1[C:17]([NH:18][CH2:19][C:20]2[CH:25]=[N:24][CH:23]=[CH:22][N:21]=2)=[C:16]([S:28][C:27]([F:31])([F:30])[F:26])[CH:15]=[N:14]1

Komponenten

5

Edukt 3

HCID 67900Methanesulfenyl chloride, trifluoro-HCID 516892Sodium BicarbonateHCID 22591646HCID 22591646, Verbindung

Produkt 1

HCID 22591644HCID 22591644, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of 3.0 g of 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylmethylamino)pyrazole dissolved in 30 ml of dried methylene chloride under a nitrogen atmosphere was added 14 ml of dried methylene chloride solution of trifluoromethylsulfenyl chloride at room temperature over about 1 hour, followed by stirring overnight. Saturated aqueous sodium hydrogen carbonate solution was added thereto, and the organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and water several times. Thereafter, the layer was purified by a silica gel column chromatography. After removal of solvent, drying in vacuo afforded 3.59 g of 1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfenyl-5-(pyrazin-2-ylmethylamino)pyrazole.

Aufarbeitung

  1. washthe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and water several times
  2. customThereafter, the layer was purified by a silica gel column chromatography
  3. customAfter removal of solvent
  4. customdrying in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bd89ebcad29448aa87d9d887ef9be4bb
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06849633B2

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