Reaktionsgleichung
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11](Cl)=[O:12])=[CH:6][CH:5]=1)[CH3:2].[Cl-].[Al+3].[Cl-].[Cl-].[CH2:18]=[CH2:19]>ClCCl>[CH2:1]([O:3][C:4]1[CH:9]=[C:8]2[C:7](=[CH:6][CH:5]=1)[CH2:10][C:11](=[O:12])[CH2:19][CH2:18]2)[CH3:2]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
39.1 g (0.20 mol) of 4-ethoxyphenylacetyl chloride in 200 ml of dichloromethane were added dropwise in the course of 1 hour at −78° C. to 53.4 g (0.4 mol) of aluminum chloride in 800 ml of dichloromethane. A vigorous stream of ethylene was subsequently passed in in the course of 15 minutes, and the mixture was allowed to come to room temperature and stirred for a further 3 hours. The dark red solution was cooled to 0° C. and carefully treated with 300 ml of ice-water. After phase separation, the organic phase was washed with 2N HCl (3×) and saturated sodium hydrogen carbonate solution, dried and evaporated on a rotary evaporator. After purification by column chromatography with petroleum ether/ethyl acetate (9:1, 8:2), 20.9 g (56% of theory) of a yellow syrup were obtained.
Aufarbeitung
- customwas subsequently passed in in the course of 15 minutes
- customto come to room temperature
- customAfter phase separation
- washthe organic phase was washed with 2N HCl (3×) and saturated sodium hydrogen carbonate solution
- customdried
- customevaporated on a rotary evaporator
- customAfter purification by column chromatography with petroleum ether/ethyl acetate (9:1, 8:2), 20.9 g (56% of theory) of a yellow syrup
- customwere obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-0fe0cdefbb12467cbe006d2f5dd21b98
- Quelldatensatz
- uspto-grants-2001_07
- Patentnummer
- US06265398B1
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