反应详情

A mixture of 4-benzylcyclohexanone (4.40 g, 0.023 mole), 3.67 g of potassium cyanide, 5.50 g of dimethylamine hydrochloride and 3 ml of methanol in 30 ml of saturated aqueous dimethylamine was stirred at room temperature for 3 days. The mixture was then extracted thoroughly with CH2Cl2, and the organic layer was concentrated in vacuo. The residue was dissolved in diethyl ether, and the basic material was precipitated with 2 N HCl in diethyl ether. This solid was recrystallized from methylene chloride:ethyl acetate to give 3.91 g (61%) of 4-benzyl-1-cyano-1-(dimethylamino)cyclohexane hydrochloride, m.p. 150°-154° C.

1. extractionThe mixture was then extracted thoroughly with CH2Cl2
2. concentrationthe organic layer was concentrated in vacuo
3. dissolutionThe residue was dissolved in diethyl ether
4. customthe basic material was precipitated with 2 N HCl in diethyl ether
5. customThis solid was recrystallized from methylene chloride