Reaktion #164136

Reaktionsgleichung

5-cyano-2-oxo-5-phenyl cyclohexane carboxylic acid methyl ester

acetic acid

→

4-oxo-1-phenyl-cyclohexane carbonitrile

Lösungsmittel

water

sulphuric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate (3×100 mL)
2. 2
   Waschenthe organic phase washed thoroughly with water (6×100 mL), saturated NaHCO3 solution (10×100 mL) and saturated NaCl solution (1×100 mL)
3. 3
   TrocknenAfter drying with Na2SO4 the solvent
4. 4
   workup.DISTILLATIONwas distilled off in a vacuum

Vorschrift

5-cyano-2-oxo-5-phenyl cyclohexane carboxylic acid methyl ester (16.1 g, 63 mmol) was dissolved in 10% sulphuric acid (218 mL) and conc. acetic acid (502 mL) and stirred for 21 h at 100° C. For work up the batch was carefully diluted with water (400 mL) with ice cooling, extracted with ethyl acetate (3×100 mL), the organic phase washed thoroughly with water (6×100 mL), saturated NaHCO3 solution (10×100 mL) and saturated NaCl solution (1×100 mL). After drying with Na2SO4 the solvent was distilled off in a vacuum.

Quelle