Sulfuric Acid → HCID 13364168, compound

Participants

Reaction Conditions

Reaction Steps

To 16.5 g of 1-[4,4-bis(p-fluorophenyl)cyclohexyl]-4-cyano-4-anilinopiperidine is added gradually a solution of 180 g of concentrated sulfuric acid and 20 ml of water under cooling. After the addition is complete, the resulting mixture is stirred at 70° C for 1 hour and then cooled. The reaction mixture is poured into water, and the precipitated powder is collected by filtration. Then water is added to the powder, the aqueous mixture is made alkaline with potassium carbonate, and the alkaline solution is extracted with chloroform. The extract is washed with water and dried over sodium sulfate, and the solvent is removed. The precipitated crystals are collected by filration and recrystallized from a mixture of chloroform and acetone to give 1-[4,4-bis(p-fluorophenyl)cyclohexyl]-4-carbamoyl-4-anilinopiperidine as white crystals, melting at 224°-227° C.

Provenance & Evidence