反应详情

Thirty grams (0.11 mole) of 3-(4,6-dichloro-s-triazin-2-yl)-3-azabicyclo[3.2.2]nonane is dissolved in 300 ml. of acetone and then 370 ml. of water is added followed by 20 g. (0.15 mole) of tert-octylamine. After stirring for 10 minutes, 4.4 g. (0.11 mole) of NaOH in 30 ml. of water is added over 20 minutes. The reaction is then heated to reflux for 19 hours. After cooling to room temperature, one liter of water is added, stirred for one hour and the white precipitate filtered off. The precipitate is washed with water, dried overnight, dissolved in dichloromethane and filtered through Magnesol®. The Magnesol® is then washed with dichloromethane, solvent removed in vacuo and recrystallized from dichloromethane-hexanes giving 20 g. of colorless crystals, m.p. 159°-162.5° C.

1. temperatureThe reaction is then heated
2. temperatureto reflux for 19 hours
3. stirringstirred for one hour
4. filtrationthe white precipitate filtered off
5. washThe precipitate is washed with water
6. customdried overnight
7. dissolutiondissolved in dichloromethane
8. filtrationfiltered through Magnesol®
9. washThe Magnesol® is then washed with dichloromethane, solvent
10. customremoved in vacuo
11. customrecrystallized from dichloromethane-hexanes giving 20 g