Hydrogen Bromide → 2-Bromo-3-methylcyclohexanone

HRID 1076122

Reaktionsgleichung

Reaktionsgleichung von HRID 1076122
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=[O:8])[CH2:3]1.C(Cl)(Cl)Cl.[BrH:13]>C(OCC)(=O)C>[Br:13][CH:3]1[CH:2]([CH3:1])[CH2:7][CH2:6][CH2:5][C:4]1=[O:8]

Komponenten

5

Edukt 3

HCID 260Hydrogen Bromide2×HCID 6212ChloroformHCID 115673-Methylcyclohexanone

Produkt 1

HCID 215419562-Bromo-3-methylcyclohexanone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

3-Methylcyclohexanone, 22.4 grams, contained in 250 ml. of chloroform and 50 ml. of ethyl acetate, is heated to boiling. A mixture of 98.3 grams of cupric bromide and 50 ml. of ethyl acetate is added and heated to maintain elimination of hydrogen bromide. When all of the hydrogen bromide is evolved, the mixture is heated to its reflux temperature for 15 minutes, filtered and the filtrate evaporated to a small volume. The residue is placed upon an alumina column and eluted with methylene chloride. Evaporation of the eluate yields 35.5 grams of crude 2-bromo-3-methylcyclohexanone suitable for condensation with the triazoles of Examples 1 or 2.

Aufarbeitung

  1. temperatureheated
  2. temperaturethe mixture is heated to its
  3. temperaturereflux temperature for 15 minutes
  4. filtrationfiltered
  5. customthe filtrate evaporated to a small volume
  6. washeluted with methylene chloride
  7. customEvaporation of the

Quellen und Nachweise

ORD-Eintrag
ord-d95861bcf9bd4edf8a662d1742418443
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03954981

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