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. 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 (2x), 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 | US04591586 |
| Source dataset | uspto-grants-1986_05 |
| ORD ID | ord-4eb6e9b12e734731a1217bb0d4049eef |
| Source note | uspto-grants-1986_05 |