Hydrochloric Acid → HCID 69891655, compound

Participants

Reaction Steps

15.2 g (103 mmol) of 4-cyanobenzoic acid was added to a mixture of a solution of 4 N hydrogen chloride in 200 ml of ethyl acetate and 50 ml of ethanol, and they were stirred for 5 days. The solvent was evaporated under reduced pressure. 100 ml of ethyl acetate was added to the obtained solid, and they were stirred for 30 minutes. The solid was taken by the filtration. The solid was reacted with 15.0 g (211 mmol) of pyrrolidine and 10.0 g (98.8 mmol) of triethylamine in 100 ml of ethanol as the solvent for two days. The solvent was evaporated. 40 ml of 6 N hydrochloric acid was added to the residue, and they were reacted at 85° C. for 4 hours. The solvent was evaporated, 50 ml of 1 N hydrochloric acid was added to the reaction mixture, and they were stirred for 30 minutes. The solid was taken by the filtration and then washed with 20 ml of ice/water. After the drying under reduced pressure, the title compound was obtained.

Provenance & Evidence