Acetic Acid → 1-(2,6,6-Trimethylcyclohex-3-en-1-yl)but-2-en-1-one

HRID 8564

Reaktionsgleichung

[CH3:1][CH:2]1[CH:7]=[CH:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[CH2:10][CH:11]=O.[CH:13](=O)[CH3:14].C(O)(=[O:18])C.O>C(OCCCC)(=O)C>[CH3:1][CH:2]1[CH:7]=[CH:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[C:10](=[O:18])[CH:11]=[CH:13][CH3:14]

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

In a 250 ml flask were added 30 g (0.18 mole) of 1-(2,6,6-trimethyl-3-cyclohexen-1-yl)-2-ethanone (94% purity), 12.0 g of butyl acetate, an aliquot according to Table 1 of the catalytic solution as prepared above and a quantity of co-ingredient according to Table 1. The resulting mixture was stirred at 100° C. To said mixture, 4.0 g (0.09 mole) of acetaldehyde, diluted in 10 g of butyl acetate were introduced under the surface of the liquid, over 3 hours. After the completion of the introduction the reaction was cooled to 35° C. To the cooled reaction medium were added 10 g of acetic acid and then 40 ml of water. After stirring a few minutes, the water phase was removed and the organic phase was neutralized by washing it with 25 g of 20% aqueous potassium carbonate.

Aufarbeitung

customas prepared above and a quantity
additionwere introduced under the surface of the liquid, over 3 hours
temperatureAfter the completion of the introduction the reaction was cooled to 35° C
customTo the cooled reaction medium
stirringAfter stirring a few minutes
customthe water phase was removed
washby washing it with 25 g of 20% aqueous potassium carbonate

Quellen und Nachweise

ORD-Eintrag: ord-abb76655ac01447ea0ff9d306d69fe0b
Quelldatensatz: uspto-grants-2006_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07091151B2

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