Benzoic Acid → 2-(2-Nitrophenyl)-2-oxoethyl benzoate

HRID 358652

Reaktionsgleichung

Reaktionsgleichung von HRID 358652
C(=O)([O-])[O-].[K+].[K+].[C:7]([OH:15])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.Br[CH2:17][C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[N+:26]([O-:28])=[O:27])=[O:19]>O>[C:7]([O:15][CH2:17][C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[N+:26]([O-:28])=[O:27])=[O:19])(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Komponenten

5

Edukt 3

HCID 243Benzoic AcidHCID 11430Potassium CarbonateHCID 2440252-Bromo-2'-nitroacetophenone

Produkt 1

HCID 536528172-(2-Nitrophenyl)-2-oxoethyl benzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Potassium carbonate (19 g) was added to a stirred suspension of benzoic acid (34 g) in water (600 ml) and the mixture was warmed gently on a steam bath. After 15 minutes, 2-bromo-2'-nitroacetophenone (68 g) and industrial methylated spirit (1 1) were added. The resultant mixture was heated under reflux for 2 hours, stirred without external heating for 1 0 minutes and then rapidly cooled to 0°-5° in an ice/salt bath with agitation. The mixture was kept at this temperature for 90 minutes and the product was collected by filtration and washed with water to give the novel compound 2-(2-nitrophenyl)-2-oxoethyl benzoate, m.p. 77-80°.

Aufarbeitung

  1. temperaturethe mixture was warmed gently on a steam bath
  2. temperatureunder reflux for 2 hours
  3. temperaturewithout external heating for 1 0 minutes
  4. temperaturerapidly cooled to 0°-5° in an ice/salt bath with agitation
  5. waitThe mixture was kept at this temperature for 90 minutes
  6. filtrationthe product was collected by filtration
  7. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-833cf48574ff496d9df04936ad625e33
Quelldatensatz
uspto-grants-1991_03
Patentnummer
US04997840

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