反应详情

A suspension of 4.0 g of 3-(4-piperidyl)-1,2-benzisoxazole, 3.2 g of 3-diethylaminopropyl chloride, 3.0 g of potassium iodide and 5.0 g of sodium bicarbonate in 100 ml of butanol was heated under reflux for 2 hrs, cooled to room temperature and filtered. The filitrate was washed with water and extracted with ether (3 times). The ether extracts were dried over anhydrous sodium sulfate, filtered and evaporated to give an oil. The oil was dissolved in 10 ml of acetonitrile and 4.2 g of fumaric acid was added. The mixture was stirred for 2 hrs, filtered and the filter cake was recrystallized three times from ethanol-ether to give 2.8 g (26%) of product, mp 174°-176°.

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