Reaktion #164108

Reaktionsgleichung

title compound

4-oxo-1-phenyl-cyclohexane carbonitrile

ethylene glycol

water

→

8-phenyl-1,4-dioxa-spiro[4.5]decane-8-carbonitrile

Lösungsmittel

toluol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwith reflux
2. 2
   Temperaturthe mixture was cooled
3. 3
   Waschenwashed with NaHCO3 solution and saturated NaCl solution
4. 4
   Trocknendried with Na2SO4
5. 5
   Einengenconcentrated to low volume in a vacuum

Vorschrift

The title compound of step 2 (43.3 g, 217 mmol) and ethylene glycol (27.4 g, 435 mmol) were boiled in toluol (430 mL) with the addition of p-toluol sulphonic acid (1.87 g, 10.9 mmol) at a water separator for 3 h with reflux. After the reaction had ended, the mixture was cooled, washed with NaHCO3 solution and saturated NaCl solution, dried with Na2SO4 and concentrated to low volume in a vacuum.

Quelle