Hydroxylamine HCl → HCID 59115139, Verbindung

HRID 1636019Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1636019
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=O.[Cl-].[OH:16][NH3+:17].C([O-])(=O)C.[Na+]>C(O)C.O>[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=[N:17][OH:16]

Komponenten

6

Edukt 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 27606164'-Thiomethyl-2,2,2-trifluoroacetophenone

Produkt 1

HCID 59115139HCID 59115139, VerbindungAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

49.3 g (0.224 mol) of 2,2,2-trifluoro-1-(4-methylthiophenyl)-ethanone are dissolved in 250 ml of ethanol at 80° C. To the solution are added dropwise 16.3 g (0.235 mol) of hydroxylammonium chloride and 31.2 g (0.381 mol) of sodium acetate dissolved in 125 ml of water. The reaction mixture is refluxed for 6.5 hours, and poured into ice water. Filtration of the precipitate yields 51.1 g of 2,2,2-trifluoro-1-(4-methylthiophenyl)-ethanone oxime, as a yellow solid. The crude product is used in the next reaction step without further purification.

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed for 6.5 hours
  2. filtrationFiltration of the precipitate

Quellen und Nachweise

ORD-Eintrag
ord-67383eb2b278404b91e1fdf942f3759d
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06512020B1

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