反应详情

温度

90 °C

To 40 ml of dimethylformamide was added 4.3 g 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 4.0 g of 4-(4-methoxyphenyl)piperazine dihydrochloride, 10.0 g of milled potassium carbonate, and 0.01 g potassium iodide. The mixture was stirred at 90° C. for two hrs, cooled, filtered, and the filtrate evaporated to an oil. The oil was stirred with 100 ml of water and extracted with ether. The ether extract was washed with water (2×), saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, ethereal oxalic acid was added. The precipitate was collected and dried to yield 3.0 g (44%) of product. Two recrystallizations from ethyl acetate/methanol/ether (10:1:5) gave the analytical sample, mp 188°-189° C. (dec).

1. temperaturecooled
2. filtrationfiltered
3. customthe filtrate evaporated to an oil
4. stirringThe oil was stirred with 100 ml of water
5. extractionextracted with ether
6. extractionThe ether extract
7. washwas washed with water (2×), saturated sodium chloride solution
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationAfter filtering
10. additionethereal oxalic acid was added
11. customThe precipitate was collected
12. customdried