Reaktion #164112

Reaktionsgleichung

dimethylamine

hydrochloric acid

title compound

4-dimethylaminomethyl-4-phenyl-cyclohexanone

KCN

→

1-dimethylamino-4-dimethylaminomethyl-4-phenyl-cyclohexane carbonitrile

Lösungsmittel

methanol

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with diethyl ether (3×20 mL)
2. 2
   EinengenThe ether phase was concentrated to low volume in a vacuum
3. 3
   Trocknendried over Na2SO4
4. 4
   Einengenconcentrated to low volume in a vacuum

Vorschrift

40% aqueous dimethylamine solution (12.8 mL, 21.1 mmol) was added in drops to a mixture of 4N hydrochloric acid (5 mL) and methanol (3 mL) with ice cooling. The title compound of step 6 (4.89 g, 21.1 mmol) and KCN (3.30 g, 50.7 mmol) were then added one after the other. The mixture was stirred for 3 d at RT. For work up the batch was mixed with water (10 mL) and extracted with diethyl ether (3×20 mL). The ether phase was concentrated to low volume in a vacuum, the residue was taken up in CH2Cl2, dried over Na2SO4 and concentrated to low volume in a vacuum.

Quelle