4-(Acetyloxy)-2-butanone → 2,3,6-Trimethylcyclohex-2-en-1-one

HRID 65808

Reaktionsgleichung

Reaktionsgleichung von HRID 65808
C(O[CH2:5][CH2:6][C:7](=O)[CH3:8])(=O)C.[CH3:10][O-:11].[Na+]>CO>[CH3:5][C:6]1[C:10](=[O:11])[CH:7]([CH3:8])[CH2:6][CH2:5][C:7]=1[CH3:8]

Komponenten

4

Edukt 2

HCID 1391004-(Acetyloxy)-2-butanoneHCID 10942334Sodium Methoxide

Produkt 1

HCID 30168432,3,6-Trimethylcyclohex-2-en-1-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

130 g of 1-acetoxybutan-3-one and sodium methylate solution in methanol are dripped in the course of one hour from separate supply vessels while stirring into 400 g of boiling diethyl ketone at such a rate that the reaction mixture remains constantly alkaline. A total of 190 g of a 30% by weight sodium methylate solution is used up in this way. The whole is then heated under reflux for another hour and then neutralized with glacial acetic acid. Deposited sodium acetate is filtered off and the filtrate is subjected to fractional distillation. 81 g of 2,3,6-trimethyl-2-cyclohexen-1-one is obtained as well as traces of 4-methyl-3-ethyl-2-cyclohexen-1-one. The yield with reference to 1-acetoxybutan-3-one is 59%.

Aufarbeitung

  1. customare dripped in the course of one hour
  2. customfrom separate supply vessels
  3. temperatureThe whole is then heated
  4. temperatureunder reflux for another hour
  5. filtrationDeposited sodium acetate is filtered off
  6. distillationthe filtrate is subjected to fractional distillation

Quellen und Nachweise

ORD-Eintrag
ord-6378b9e4c99d40c6811d8c8750d9496a
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128728

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