反应详情

A mixture of 5.0 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 4.0 g of 1-(4-fluorophenyl)piperazine, 10 g of potassium carbonate and a few crystals potassium iodide in 70 ml of dimethylformamide was stirred at 80° C. for 4.5 hr. The mixture was cooled, filtered and concentrated to an oil, which was stirred with water and extracted with ethyl acetate-ether. The organic extracts were washed with water (2×), saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The mixture was filtered and concentrated. The residue was purified by column chromatography (silica gel, tetrahydrofuran) to give an oil. The oil was converted to 4.5 g (45%) of product by treatment with oxalic acid. Two recrystallizations from ethyl acetate/methanol gave the analytical sample, mp 186°-187° C. (dec).

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. concentrationconcentrated to an oil, which
4. extractionextracted with ethyl acetate-ether
5. washThe organic extracts were washed with water (2×), saturated sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationThe mixture was filtered
8. concentrationconcentrated
9. customThe residue was purified by column chromatography (silica gel, tetrahydrofuran)
10. customto give an oil
11. customTwo recrystallizations from ethyl acetate/methanol
12. customgave the analytical sample, mp 186°-187° C. (dec)