反应详情

10 g. (0.025 mole) of the 4-methylbenzenesulfonate ester of example 1(b), 3.32 g. (0.027 mole) of 3-azabicyclo[3.2.2]nonane, and 3.27 g. (0.025 mole) of diisopropylethylamine are refluxed in 500 ml. of toluene for three hours. The reaction mixture is then cooled, washed with 10% KOH and water. The resulting toluene solution is shaken with 10% HCl and the resulting precipitate is filtered from the two phases. This salt is dissolved in a minimum of hot methanol, precipitated with ether, filtered, and dried at 80° under vacuum to yield 4.45 g. of 2-[2-(3-azabicyclo[3.2.2]nonan-3-yl)ethyl]-1H-benz[de]isoquinoline-1,3(2H)-dione, hydrochloride (1:1); m.p. 301°-302° (dec.).

1. temperatureThe reaction mixture is then cooled
2. washwashed with 10% KOH and water
3. filtrationthe resulting precipitate is filtered from the two phases
4. dissolutionThis salt is dissolved in a minimum of hot methanol
5. customprecipitated with ether
6. filtrationfiltered
7. customdried at 80° under vacuum
8. customto yield 4.45 g