反应详情

温度

90 °C

To 40 ml of dimethylformamide was added 4.06 g of 4-(3-phenylpropyl)piperidine, 3.4 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 10 g of milled potassium carbonate, and 0.01 g of potassium iodide. After stirring at 90° C. for three hrs, the mixture was cooled, filtered and the filtrate was evaporated to an oil. The oil was stirred with 100 ml of water for ten mins and then extracted with ether. The ether extract was washed with water (2x), saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, the solution was acidified to pH 1 with ethereal hydrogen chloride. The resultant precipitate was collected and dried to give 5.0 g (60%) of product, mp 95° C. Recrystallization from ethyl acetate/methanol (5:1) gave the analytical sample, mp 136°-137° C.

1. temperaturethe mixture was cooled
2. filtrationfiltered
3. customthe filtrate was evaporated to an oil
4. stirringThe oil was stirred with 100 ml of water for ten mins
5. extractionextracted with ether
6. extractionThe ether extract
7. washwas washed with water (2x), saturated sodium chloride solution
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationAfter filtering
10. customThe resultant precipitate was collected
11. customdried