HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58424845, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | HCID 58424857 | HCID 58424857 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58424845 | HCID 58424845 | 64% |
Reaction Steps
The compound (55 mg, 0.146 mmol) prepared in step 3 was dissolved in N,N-dimethylformamide (3 ml), sequentially added with palladium(II) acetate (9.83 mg, 0.0438 mmol), 1,3-bis(dephenylphosphino)propane (18 mg, 0.0438 mmol), tributylphosphine (0.036 ml, 0.146 mmol), and potassium carbonate (40 mg, 0.292 mmol). The resulting mixture was refluxed for 5 hours. Water was added to the above solution and the mixture was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and concentrated to dryness. The residue was then purified by flash column chromatography (hexane:ethyl acetate=3:1) to obtain title compound (31 mg, yield: 64%, white solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815891B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-b2ed582c81384b029075317714809bae |
| Source note | uspto-grants-2014_08 |