Potassium Carbonate → HCID 88426431, Verbindung

HRID 465988Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 465988
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:10]=2)=O)[CH:2]=1.[Cl-].[OH:27][NH3+:28].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7](=[N:28][OH:27])[C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:10]=2)[CH:2]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 21645Hydroxylamine HClHCID 149893984-Chloro-N-[3-(pyridine-3-carbonyl)phenyl]benzene-1-sulfonamide

Produkt 1

HCID 88426431HCID 88426431, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

7.45 g (20 mmol) of the compound from Example 1, 2.08 g (30 mmol) of hydoxylammonium chloride and 4.14 g (30 mmol) of potassium carbonate are refluxed in 20 ml of ethanol for 15 h. After cooling to room temperature, the mixture is evaporated and the residue is stirred in 50 ml of water for 3 h (after this time no oily residues, but only crystalline residues, were still undissolved). The precipitate was filtered off, washed with water and recrystallised from methanol by addition of water. Yield: 5.71 g (73.7% of theory) M.p.: 170° C.

Aufarbeitung

  1. customthe mixture is evaporated
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. customrecrystallised from methanol by addition of water

Quellen und Nachweise

ORD-Eintrag
ord-718d871338834745b711958b6d497b62
Quelldatensatz
uspto-grants-1992_10
Patentnummer
US05155121

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