Hydrochloric Acid → 1-(2-Hydroxyphenyl)ethanone oxime

HRID 1293100Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1293100
[Cl-].[OH:2][NH3+:3].[C:4]([O-:7])(=O)[CH3:5].[Na+].O[CH2:10][C:11]([C:13]1C=C[CH:16]=[CH:15][CH:14]=1)=O.Cl>C(O)C.O>[OH:7][C:4]1[CH:5]=[CH:16][CH:15]=[CH:14][C:13]=1[C:11](=[N:3][OH:2])[CH3:10]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 21645Hydroxylamine HClHCID 68490alpha-HydroxyacetophenoneHCID 517045Sodium Acetate

Produkt 1

HCID 1020211-(2-Hydroxyphenyl)ethanone oxime

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 19096565Water ethanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

Hydroxylammoniumchloride (6.96 g, 100 mmol) and sodium acetate. 3H2O (13.6 g, 100 mmol) were dissolved in 150 mL ethanol:water (7:3) and added to a solution of 2-hydroxyacetophenone (6.81 g, 50 mmol) in 50 mL ethanol:water (7:3). The pH was adjusted to 4–5 with 4N HCl (˜10 mL) and the reaction mixture was then heated to reflux (100° C.) for 1 hour. The oil bath was removed and the mixture was left overnight with stirring. Ethanol was partly removed by evaporation and the aqueous phase was extracted with ethyl acetate two times. The combined organic phases were dried over magnesium sulphate and evaporated to dryness to produce 7.55 g of pure 24.

Aufarbeitung

  1. temperaturethe reaction mixture was then heated
  2. customThe oil bath was removed
  3. customEthanol was partly removed by evaporation
  4. extractionthe aqueous phase was extracted with ethyl acetate two times
  5. dry with materialThe combined organic phases were dried over magnesium sulphate
  6. customevaporated to dryness
  7. customto produce 7.55 g of pure 24

Quellen und Nachweise

ORD-Eintrag
ord-0a92466deaa0426a89a4ad5b758e9eaa
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07238713B2

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