反应详情

A suspension of 4.5 g of 3-(4-piperidyl)-1,2-benzisoxazole, 2.6 g of 2-dimethylaminoethyl chloride, 3.0 g of potassium iodide and 5.0 g of potassium carbonate in 100 ml of butanol was heated under reflux for 2 hrs, cooled to room temperature and filtered. The filtrate was washed with water and extracted with ether (3 times). The ether extracts were dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure to give an oil. The oil was dissolved in 10 ml of acetonitrile and 3.2 g of fumaric acid was added. The reaction mixture was stirred for 2 hrs, filtered and the filter cake was recrystallized three times from ethanol-ether to give 2.2 g (19.8%) of product, mp, 215°-217°.

1. temperaturewas heated
2. temperatureunder reflux for 2 hrs
3. filtrationfiltered
4. washThe filtrate was washed with water
5. extractionextracted with ether (3 times)
6. dry with materialThe ether extracts were dried over anhydrous sodium sulfate
7. customthe solvent was removed under reduced pressure
8. customto give an oil
9. filtrationfiltered
10. customthe filter cake was recrystallized three times from ethanol-ether