反应详情

温度

90 °C

To 50 ml of dimethylformamide was added 2.6 g of 4-(2-hydroxyethyl)piperazine, 6.4 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 10.0 g of milled potassium carbonate, and 0.01 g of potassium iodide. The mixture was stirred at 90° C. for five hrs, cooled, filtered, and evaporated to an oil. The oil was stirred with 100 ml water for ten mins, 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 hydrogen chloride was added, and the precipitate was collected and dried to give 4.3 g (57%) of product. Two recrystallizations from ethyl acetate/methanol, gave the analytical sample, mp 228° C. (dec).

1. temperaturecooled
2. filtrationfiltered
3. customevaporated to an oil
4. stirringThe oil was stirred with 100 ml water for ten mins
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 hydrogen chloride was added
11. customthe precipitate was collected
12. customdried