Benzene → HCID 14137252, Verbindung

HRID 1075955

Reaktionsgleichung

Reaktionsgleichung von HRID 1075955
[CH3:1][C@H:2]1[CH2:8][C:6](=[O:7])[C@H:5]([CH:9]([CH3:11])[CH3:10])[CH2:4][CH2:3]1.[CH3:12][C:13]([CH:15]=[CH2:16])=[O:14].C1C=CC=CC=1.C([O-])(=O)C.[Na+]>O.C(O)(=O)C>[CH3:1][CH:2]1[CH2:3][CH2:4][CH:5]([CH:9]([CH3:11])[CH3:10])[C:6](=[O:7])[CH:8]1[CH2:16][CH2:15][C:13](=[O:14])[CH3:12]

Komponenten

7

Edukt 4

HCID 241BenzeneHCID 6570Methyl vinyl ketoneHCID 26447MenthoneHCID 517045Sodium Acetate

Produkt 1

HCID 14137252HCID 14137252, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 19.6 g of the pyrrolidine-enamine of p-menthone, 10 ml of methylvinyl ketone and 150 ml of anhydrous benzene is refluxed under nitrogen for 20 hours. The mixture is then cooled and treated with 6 g of sodium acetate in 12 ml of water as well as with 12 ml of acetic acid. The mixture is again refluxed for 4 hours. Then, the product is extracted with benzene and the solvent evaporated. The residue is fractionated in vacuo and there is obtained 1-methyl-4-isopropyl-2-(3'-oxobutyl)-cyclohexan-3-one with a boiling point of 88°-90°C.

Aufarbeitung

  1. temperatureis refluxed under nitrogen for 20 hours
  2. temperatureThe mixture is then cooled
  3. temperatureThe mixture is again refluxed for 4 hours
  4. extractionThen, the product is extracted with benzene
  5. customthe solvent evaporated

Quellen und Nachweise

ORD-Eintrag
ord-dbcb3ab2762a4a3b8b44db6097bd1fa6
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03954794

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