Potassium Carbonate → HCID 2772320, compound

Participants

Reaction Steps

A mixture of 4.07 g (0.0225 mol) of DL-camphorimide (II), 6.71 g (0.0225 mol) of 8-(2-pyridyl)-8-aza-5-azoniaspiro[4,5]-decane bromide (III) and 3.73 g (0.027 mol) of potassium carbonate was refluxed in 80 ml of absolute dimethylformamide for 24 hours, then the resulting mixture was cooled, filtered, and dimethylformamide was distilled off under reduced pressure. The residue was dissolved in 100 ml of 5% HCl, the resulting solution was extracted twice with 50 ml of ether to remove impurities of non-basic nature, and saturated with soda. The precipitated base was extracted with ethyl acetate, the extract was dried with potassium carbonate and purified by passing through a column packed with a neutral aluminum oxide 5 cm thick (with ethyl acetate as eluent). After the solvent was distilled off, there was obtained a free base in the form of an oil which was then crystallized. Mp. 96°-97° C.

Provenance & Evidence