反应详情

To 21.7 g of 2-azacyclotridecanone in 200 ml of dry benzene was added dropwise 15.3 g of phosphorus oxychloride. The mixture was stirred at room temperature for 4 hours after which 19.8 g of cis-2-phenylcyclopentylamine hydrochloride was added. The reaction mixture was stirred at room temperature for 2 hours and refluxed for 24 hours. The resulting homogeneous solution was washed with 2 N NaOH, 2 N HCl and saturated NaCl solution, dried over sodium sulfate and the solvent evaporated. The resulting oily product crystallized from acetone and was recrystallized from methanol-acetone to give the desired product, M.P. 156°-159° C.

1. additionwas added
2. temperaturerefluxed for 24 hours
3. washThe resulting homogeneous solution was washed with 2 N NaOH, 2 N HCl and saturated NaCl solution
4. dry with materialdried over sodium sulfate
5. customthe solvent evaporated
6. customThe resulting oily product crystallized from acetone
7. customwas recrystallized from methanol-acetone