反应详情

A mixture of 15 g of 1,4-dioxa-8-azaspiro-[4.5]decane, 25 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 29 g of potassium carbonate and a few crystals potassium iodide in 80 ml of dimethylformamide was stirred at 70°-75° C. in two hrs. The mixture was cooled, filtered, and concentrated to an oil. The oil was stirred with water and extracted with ether. The organic extracts were washed with water (2×), saturated sodium chloride solution, dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was treated with ethereal hydrogen chloride to give 18 g (48%) or product, mp 170°-173° C. Recrystallization from ethyl acetate/methanol gave the analytical sample, mp 178°-179° C.

1. temperatureThe mixture was cooled
2. filtrationfiltered
3. concentrationconcentrated to an oil
4. extractionextracted with ether
5. washThe organic extracts were washed with water (2×), saturated sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. additionThe residue was treated with ethereal hydrogen chloride
10. customto give 18 g (48%) or product, mp 170°-173° C
11. customRecrystallization from ethyl acetate/methanol
12. customgave the analytical sample, mp 178°-179° C.