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. for 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.