HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58424897, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | HCID 58424921 | HCID 58424921 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58424897 | HCID 58424897 | 77.3% |
Reaction Steps
The compound (1.11 g, 2.94 mmol) prepared in step 5 was dissolved in N,N-dimethylformamide (10.0 ml), added with palladium(II) acetate (215 mg, 0.881 mmol), 1,3-bis(dephenylphosphino)propane (363 mg, 0.881 mmol), tributylphosphine (0.724 ml, 2.94 mmol), and potassium carbonate (812 mg, 5.87 mmol). The resulting mixture was refluxed for 3 hours and cooled to room temperature. Water and dichloromethane were added and the mixture was extracted. The organic layer was dried over anhydrous magnesium sulfate and concentrated to dryness. The residue was then purified by flash column chromatography (dichloromethane:ethyl acetate=4:1) to obtain the title compound (776.5 mg, yield: 77.3%, white solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815891B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-cf36ee18047148ac9f6097141f01136e |
| Source note | uspto-grants-2014_08 |