HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Iodide → 8-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-1,4-dioxa-8-azaspiro[4.5]decane hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| Reactant | 3-(3-Chloropropyl)-6-fluorobenzo[d]isoxazole | HCID 10910880 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 8-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-1,4-dioxa-8-azaspiro[4.5]decane hydrochloride | HCID 23315786 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04524209 |
| Source dataset | uspto-grants-1985_06 |
| ORD ID | ord-749a08fdd8644ce2908811f6ae80bd81 |
| Source note | uspto-grants-1985_06 |