(3,5-Difluorophenyl)hydrazine → HCID 18951060, Verbindung

HRID 2248267Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2248267
[F:1][C:2]1[CH:3]=[C:4]([NH:9]N)[CH:5]=[C:6]([F:8])[CH:7]=1.[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([S:18]([NH:21][CH:22]2[CH2:27][CH2:26][C:25](=O)[CH2:24][CH2:23]2)(=[O:20])=[O:19])=[CH:14][CH:13]=1>C(O)C.S(=O)(=O)(O)O.O>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([S:18]([NH:21][CH:22]2[CH2:23][C:24]3[C:3]4[C:4](=[CH:5][C:6]([F:8])=[CH:7][C:2]=4[F:1])[NH:9][C:25]=3[CH2:26][CH2:27]2)(=[O:20])=[O:19])=[CH:14][CH:13]=1

Komponenten

6

Edukt 2

HCID 2774213(3,5-Difluorophenyl)hydrazineHCID 14130443HCID 14130443, Verbindung

Produkt 1

HCID 18951060HCID 18951060, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittelHCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

14.0 g (97 mmol) of the compound of Example I and 27.95 g (97 mmol) of 4-chloro-N-(4-oxo-cyclohexyl)benzenesulphonamide are refluxed for 5 hours in 190 ml of ethanol and 36 ml of concentrated sulphuric acid, then the mixture is cooled and diluted with 300 ml of water. The mixture is extracted 4 times using 250 ml of ethyl acetate each time, and the organic phase is dried using sodium sulphate, filtered with suction over kieselguhr and evaporated. The residue is stirred with methylene chloride and dried in a high vacuum.

Aufarbeitung

  1. extractionThe mixture is extracted 4 times
  2. customthe organic phase is dried
  3. filtrationfiltered with suction over kieselguhr
  4. customevaporated
  5. customdried in a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b16b6b12cb1a418e82a3669b5656097f
Quelldatensatz
uspto-grants-1991_08
Patentnummer
US05039670

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