反应详情

温度

80 °C

To 35 ml of dimethylformamide was added 4.06 g of 4-acetyl-4-phenylpiperidine, 5.0 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 10 g of milled anhydrous potassium carbonate, and a few crystals of potassium iodide. After stirring at 80° C. for two hrs, the mixture was filtered. The filtrate was evaporated and the residue was stirred with 100 ml of water and then extracted into ether. The ether solution was washed with water (2x), saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, the solution was acidified with ethereal hydrogen chloride and the resultant precipitate was collected and dried to yield 5.5 g (66%) of product, mp 170° C. (dec). Three recrystallizations from ethyl acetate:methanol (9:1) gave the analytical sample, mp 200°-203° C.

1. filtrationthe mixture was filtered
2. customThe filtrate was evaporated
3. stirringthe residue was stirred with 100 ml of water
4. extractionextracted into ether
5. washThe ether solution was washed with water (2x), saturated sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationAfter filtering
8. customthe resultant precipitate was collected
9. customdried