HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 17906297, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | (~2~H_11_)Piperidine | HCID 16212919 | — |
| Reactant | HCID 17906318 | HCID 17906318 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 17906297 | HCID 17906297 | 73.9% |
Reaction Steps
Combine 3-[4-(2-bromo-ethoxy)-phenyl]-6-fluoro-benzo[d]isoxazole (550 mg, 1.63 mmol), potassium carbonate (500 mg, 3.62 mmol), piperidine- d11 (630 mg, 6.55 mmol) and 5% aqueous acetonitrile. Under a nitrogen atmosphere, heat to reflux overnight. Cool to room temperature and pour the reaction mixture into water resulting in white solid precipitation. Collect the solid and dry in vacuo. Dissolve the solid in ethyl acetate and filter to remove the insoluble materials and concentrate in vacuo. Take the solid up in diethyl ether, filter and precipitate the hydrochloride salt out of solution by addition of hydrogen chloride in diethyl ether. Collect the desired salt and dry in vacuo to give the title compound as a solid (410 mg, 67% Yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253165B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-3a9d5c40a17549d5ab1af4fcb143ce18 |
| Source note | uspto-grants-2007_08 |