Piperidine → 1-Piperidinecarbodithioic acid, compd. with piperidine (1:1)

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Reaction Steps

Carbon bisulfide is then added to the solution at a temperature of 13°-27° C. The reaction of piperidine and carbon bisulfide is also exothermic. The temperature will rise at least 15° C. The solution is stirred at 13°-27° C. for 15 minutes. To stir longer than 15 minutes is not harmful, but will extend the time cycle unnecessarily. At these temperatures, the reaction is incomplete because some of the carbon bisulfide is absorbed on the surface of the 1-piperidine-carbodithioic acid piperidinium salt and does not react with the piperidine. At this point, the reaction solution is heated to above the boiling point of carbon bisulfide, preferably 52°-56° C. over 1-2 hours and held at 52°-56° C. for 1/2 hour. To hold the solution at this temperature range for up to one hour is not harmful but will extend the time cycle unnecessarily. At these temperatures, the vapors of carbon bisulfide leave the surface of the 1-piperidine-carbodithioic acid piperidine salt particles in suspension. As the carbon bisulfide vapors pass through the water solution of piperidine, they react with the remaining piperidine and the reaction is completed.

Provenance & Evidence