Hydrochloric Acid → HCID 67198201, compound

Participants

Reaction Steps

A mixture of 37.04 g ethyl 4-{1-[2-(4-chloro-2,5-difluorophenyl)-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl]piperidin-4-yl}butanoate, 160 ml of 1M aqueous sodium hydroxide, and 400 ml of THF-EtOH (1:1) was stirred at ambient temperature for 4 hours. To the reaction mixture, 160 ml of 1M hydrochloric acid aqueous solution and 700 ml of water were added, and the mixture was extracted twice with chloroform. The organic phase obtained was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The solid obtained was dissolved in 300 ml of THF, 50 ml of 4M HCl-EtOAc solution was added, the solution was concentrated under reduced pressure, and the resultant solid was recrystallized from water-acetonitrile to yield 25.35 g of 4-{1-[2-(4-chloro-2,5-difluorophenyl)-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl]piperidin-4-yl}butanoic acid hydrochloride.

Provenance & Evidence