HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 21960068, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Bromoethyl methyl ether | HCID 80972 | — |
| 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 21960068 | HCID 21960068 | — |
Reaction Steps
A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.75 g, 17 mmol), K2CO3 (3 g, 21.7 mmol), bromoethyl methyl ether (2.84 g, 20.4 mmol) in acetonitrile (150 ml) was heated at reflux for 3.5 hours. The reaction was cooled. The inorganics were filtered and rinsed with DCM. The organic solution was concentrated down to an oil (7 g). Purification on a flash chromatography column (SiO2, 45 g; eluted with methanol/DCM) gave a light yellow oil as product (4 g, 87%). This oil was dissolved into ethanol and treated with a solution of fumaric acid (1.67 g) in ethanol (20 ml). White crystals (5.15 g) were collected, m.p.=157°-158° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05607945 |
| Source dataset | uspto-grants-1997_03 |
| ORD ID | ord-097702d2c3214563b9475e0f7e686755 |
| Source note | uspto-grants-1997_03 |