Thionyl Chloride → Ethyl (2-chloro-6-oxocyclohex-1-en-1-yl)acetate
Reaktionsgleichung
O.[O:2]=[C:3]1[CH2:8][CH2:7][CH2:6][C:5](=O)[CH:4]1[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12].S(Cl)([Cl:18])=O>C(Cl)Cl>[Cl:18][C:5]1[CH2:6][CH2:7][CH2:8][C:3](=[O:2])[C:4]=1[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A slurry of ethyl α-(2,6-dioxocyclohexyl)acetate hydrate (1.53 kg) in methylene chloride (7.7L) is brought to reflux and then thionyl chloride (1.80 kg) is added dropwise over a period of 1.75 hours. The solution is refluxed for 3 hours and then evaporated in vacuo to yield an oil which is distilled to give ethyl α-(2-chloro-6-oxocyclohex-1-enyl)acetate as a yellow oil, bp 115°-125°/0.2 mm.
Aufarbeitung
- temperatureto reflux
- temperatureThe solution is refluxed for 3 hours
- customevaporated in vacuo
- customto yield an oil which
- distillationis distilled
Quellen und Nachweise
- ORD-Eintrag
- ord-852f04908fb64e259b45c1c4b91b9d43
- Quelldatensatz
- uspto-grants-1989_01
- Patentnummer
- US04801605
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