Hydroxylamine HCl → HCID 57353441, Verbindung

HRID 1636013

Reaktionsgleichung

Reaktionsgleichung von HRID 1636013
[F:1][C:2]([F:13])([F:12])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][CH:6]=1)=O.[Cl-].[OH:15][NH3+:16].C([O-])(=O)C.[Na+]>C(O)C.O>[F:1][C:2]([F:13])([F:12])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][CH:6]=1)=[N:16][OH:15]

Komponenten

6

Edukt 3

HCID 21645Hydroxylamine HClHCID 1362374-(Trifluoroacetyl)tolueneHCID 517045Sodium Acetate

Produkt 1

HCID 57353441HCID 57353441, VerbindungAusbeute 73,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

49.5 g (0.263 mol) of 2,2,2-trifluoro-1-(4-methylphenyl)-ethanone are dissolved in 250 ml of ethanol at 80° C. To the solution are added dropwise 19.2 g (0.276 mol) of hydroxylammonium chloride and 36.7 g (0.447 mol) of sodium acetate dissolved in 125 ml of water. The reaction mixture is refluxed for 3.5 hours. The mixture is poured into ice water, affording a white solid. The filtration yields 39.2 g of 2,2,2-trifluoro-1-(4-methylphenyl)-ethanone oxime as a white solid, mp. 54-68° C. The crude product is used in the next step without further purification.

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed for 3.5 hours
  2. customaffording a white solid
  3. filtrationThe filtration

Quellen und Nachweise

ORD-Eintrag
ord-ecf269ff19ff4f64b84ccb3d7bd6fb1c
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06512020B1

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