反应详情

To 43.5 g (0.22 mole) of 2-azacyclotridecanone in 200 ml of dry benzene is added dropwise 30.7 g (0.2 mole) of phosphorousoxychloride. The reaction mixture is stirred at room temperature for 4 hours after which 33.8 g (0.2 mole) of o-biphenylamine is added and stirring is continued at room temperature for 1 hour then at reflux temperature for 4 hours. The reaction mixture is alowed to stand overnight then is washed with 2N hydrochloric acid, dried and evaporated leaving a residue which is recrystallized from acetone/methanol to give 2-(o-biphenylylimino)azacyclotridecane hydrochloride, M.P. 249°-251° C.

1. additionis added
2. temperatureat reflux temperature for 4 hours
3. waitto stand overnight
4. washthen is washed with 2N hydrochloric acid
5. customdried
6. customevaporated
7. customleaving a residue which
8. customis recrystallized from acetone/methanol