反应详情

A mixture of 4.1 g of 4,4-diphenylcyclohexyl tosylate, 2.8 g of 4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol, 1.1 g of sodium carbonate and 400 ml of toluene is stirred under reflux for 48 hours. The reaction mixture is concentrated completely under reduced pressure, water is added to the residue, and the aqueous mixture is extracted with chloroform. The extract is washed with water and dried over sodium sulfate, and the solvent is removed. The esidual viscous oil is purified by column chromatography on silica gel using chloroform and then chloroform - methanol (9:1) as an eluent. The purified base is converted in a conventional manner into the hydrochloride. Thus is obtained 1-(4,4-diphenylcyclohexyl)-4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol hydrochloride monohydrate as white crystals, melting at 270°-273° C.

1. temperatureunder reflux for 48 hours
2. concentrationThe reaction mixture is concentrated completely under reduced pressure, water
3. additionis added to the residue
4. extractionthe aqueous mixture is extracted with chloroform
5. washThe extract is washed with water
6. dry with materialdried over sodium sulfate
7. customthe solvent is removed
8. customThe esidual viscous oil is purified by column chromatography on silica gel