Benzenesulfonic Acid → HCID 86622716, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of 4-[4-(3,4-dichloro-2-methyl-phenoxy)-piperidin-1-ylmethyl]-piperidine-1-carboxylic acid tert-butyl ester (120 g) and ethanol (600 mL) were heated to 75° C. to give a solution. Benzenesulfonic acid (70% in water, 144.2 g) in ethanol (120 mL) was added dropwise over 45 min followed by a rinse with ethanol (60 mL). The solution was heated at 75° C. for 1 h and was then cooled to 20° C. over 1 h 45 min. The resultant solid was collected, the filter cake was washed with ethanol (480 mL) then dried under vacuum overnight at 40° C. to give 4-[4-(3,4-dichloro-2-methyl-phenoxy)-piperidin-1-ylmethyl]-piperidine di-benzenesulfonate salt as a white solid (161.9 g).

Provenance & Evidence