HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 21959990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ethyl 2-bromopropionate | HCID 79040 | — |
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | 3-(4-Piperidyl)-6-fluoro-1,2-benzisoxazole | HCID 849421 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 21959990 | HCID 21959990 | — |
Reaction Steps
A mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (5 g, 22.7 mmol), K2CO3 (3.8 g, 27.5 mmol) and ethyl bromopropionate (5 g, 27.6 mmol, 1.2 eq) in acetonitrile (200 ml) was heated at reflux for 16 hours. The mixture was cooled and filtered. The solvent was removed, and the residue was purified on a flash chromatography column (60 g, SiO2, eluted with DCM). The material thus purified weighed 7.27 g (83%). The fumarate salt was prepared by treatment of the free base (2.17 g) with fumaric acid (820 mg, 1.0 eq) in ethanol. Recrystallization from ethanol yielded 2.49 g of white crystals, m.p.=135°-136° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05559117 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-b4a1ff74c52640979ed7d65b7b361715 |
| Source note | uspto-grants-1996_09 |