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Benzoic Acid → 3-Oxobutan-2-yl benzoate

HRID 1290822
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1290822
Cl[CH:2]([CH3:6])[C:3](=[O:5])[CH3:4].[C:7]([OH:15])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(N(CC)CC)C>C(#N)C>[C:7]([O:15][CH:2]([CH3:6])[C:3](=[O:5])[CH3:4])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 243Benzoic AcidHCID 8471TriethylamineHCID 200263-Chloro-2-butanone

Produkt 1

HCID 2319833-Oxobutan-2-yl benzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of 3-chlorobutanone (10.6 g), benzoic acid (15.0 g), triethylamine (30 ml) and acetonitrile (100 ml) was heated under reflux for 1 hour 30 minutes. The mixture was cooled and filtered to remove precipitated triethylamine hydrochloride. The acetonitrile was removed from the filtrate under reduced pressure and the residue dissolved in ethyl acetate and washed with water. The organic extracts were dried over magnesium sulphate, filtered over active carbon and the solvent was removed from the filtrate under reduced pressure, to give a yellow oil of 3-benzoyloxybutan-2-one. Yield 16.7 g. The oil was used directly without further purification in the next step.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour 30 minutes
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. customto remove
  6. customprecipitated triethylamine hydrochloride
  7. customThe acetonitrile was removed from the filtrate under reduced pressure
  8. dissolutionthe residue dissolved in ethyl acetate
  9. washwashed with water
  10. dry with materialThe organic extracts were dried over magnesium sulphate
  11. filtrationfiltered over active carbon
  12. customthe solvent was removed from the filtrate under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9b21958bae674b96a195899ade3e7919
Quelldatensatz
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05753665

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