Hydrochloric Acid → 4-Benzyl-4-(dimethylamino)cyclohexanone

Participants

Reaction Steps

200 ml hydrochloric acid (32 wt. %) were diluted with 120 ml water, 78.4 g crude (8-benzyl-1,4-dioxa-spiro[4.5]dec-8-yl)-dimethyl-amine were added to this approx. six molar hydrochloric acid and the mixture was stirred for 24 hours. The reaction mixture was washed three times with 100 ml diethyl ether each time, rendered alkaline (pH>10) with 100 ml sodium hydroxide solution (32 wt. %), while cooling on an ice-bath, and extracted three times with 100 ml methylene chloride each time. The extracts were combined, dried over sodium sulfate and filtered and the filtrate was concentrated. 50.4 g 4-benzyl-4-dimethylamino-cyclohexanone were obtained.

Provenance & Evidence