Sodium Carbonate → Hydrochloric Acid

Participants

Reaction Steps

A mixture of 4.9 g. (0.02 mole) of 8-[3-chloro-1-propyl)-8-azaspiro[4.5]decane-7.9-dione, 3.3 g. (0.02 mole) prepared in the manner of U.S. Pat. No. 3,398,151, N-(2-pyrimidyl)piperazine, and 2.2 g. (0.02 mole) of sodium carbonate in 75 ml. of n-butanol is refluxed for three days and filtered. The filtrate is concentrated in vacuo and the residue taken up in 100 ml. of benzene. Addition of 4.0 ml. of 5.0 N ethanolic hydrogen chloride to the benzene solution of the free base provides the product 8-[3-[4-(2-pyrimidinyl)-1-piperazinyl]propyl]-8-azaspiro[4.5]decane-7,9-dione as a hydrochloride salt which is collected and crystallized from absolute ethanol-ether, yield 3.4 g., m.p. 214°-215°C. (corr.).

Provenance & Evidence