反应详情

To 40 ml of dimethylformamide was added, 5.0 g of 1-(2-chlorophenyl)piperazine hydrochloride hydrate, 6.4 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 10 g of milled potassium carbonate, and 0.01 g of potassium iodide, and the mixture was stirred at 90° C. for 2 hrs. The mixture was cooled, filtered and the filtrate evaporated to an oil. The oil was stirred with 100 ml water for five mins and then extracted with ether. The ether extract was washed with water (2×), saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. After filtering, the solution was acidified to pH 1 with ethereal hydrogen chloride, and the precipitate was collected and dried to give 5.7 g (70%) of product, mp 195° C. (dec). Two recrystallizations from ethyl acetate/methanol (5:1) gave the analytical sample, mp 228° C. (dec).

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. customthe filtrate evaporated to an oil
4. extractionextracted with ether
5. extractionThe ether extract
6. washwas washed with water (2×), saturated sodium chloride solution
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationAfter filtering
9. customthe precipitate was collected
10. customdried