反应详情

To 28.3 g (0.223 mole) of an enantholactam in 250 ml of benzene is added 34.1 g (0.223 mole) of phosphorous oxychloride over 30 minutes. The mixture is stirred at room temperature for 4 hours after which 41.2 g (0.223 mole) of dodecylamine is added. The reaction mixture is stirred at room temperature for 1 hour and refluxed for 4 hours then allowed to stand overnight. The resulting precipitate is washed with benzene, and the benzene wash is extracted with aqueous 2 N hydrochloric acid and combined with the precipitate. The combined fractions are made alkaline with 2N sodium hydroxide, extracted into ether-methylene chloride, dried and recrystallized from isopropyl alcohol to give 2-dodecyliminooctahydroazocine.

1. additionis added
2. temperaturerefluxed for 4 hours
3. waitto stand overnight
4. washThe resulting precipitate is washed with benzene
5. washthe benzene wash
6. extractionis extracted with aqueous 2 N hydrochloric acid
7. extractionextracted into ether-methylene chloride
8. customdried
9. customrecrystallized from isopropyl alcohol