Hydroxylamine HCl → HCID 73455958, Verbindung

HRID 1636016Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1636016
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:6]=1C)=O.[Cl-].[OH:16][NH3+:17].[C:18]([O-])(=O)C.[Na+]>C(O)C.O>[F:14][C:2]([F:1])([F:13])[C:3]([C:5]1[CH:6]=[CH:7][C:8]([CH3:18])=[CH:9][C:10]=1[CH3:11])=[N:17][OH:16]

Komponenten

6

Edukt 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 186745371-(2,6-Dimethylphenyl)-2,2,2-trifluoroethan-1-one

Produkt 1

HCID 73455958HCID 73455958, VerbindungAusbeute 88,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

12.6 g (0.062 mol) of 2,2,2-trifluoro-1-(2,6-dimethylphenyl)-ethanone are dissolved in 30 ml of ethanol at 80° C. To the solution are added dropwise 4.6 g (0.066 mol) of hydroxylammonium chloride and 8.7 g (0.106 mol) of sodium acetate dissolved in 15 ml of water. The reaction mixture is refluxed overnight, affording white precipitation. The mixture is poured into ice water, and extracted with ethyl acetate. The organic phase is washed with water, NH4Cl aq, and brine, dried over MgSO4, and concentrated, yielding 11.9 g of crude 2,2,2-trifluoro-1-(2,4-dimethylphenyl)-ethanone oxime as a colorless liquid. The crude product is used in the next reaction step without further purification.

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed overnight
  2. customaffording white
  3. customprecipitation
  4. additionThe mixture is poured into ice water
  5. extractionextracted with ethyl acetate
  6. washThe organic phase is washed with water, NH4Cl aq, and brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-7c0bee1dc5584a8593ed51b729c955da
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06512020B1

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