Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| Reactant | HCID 66920372 | HCID 66920372 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66920386 | HCID 66920386 | 63.8% |
Reaction Steps
A mixture of the compound of example 26, step 2, (100 mg, 0.16 mmol), triethylamine (166 mg, 1.6 mmol), 1,3-bis(diphenylphosphino)propane (7.4 mg, 18 μmol) and palladium(II) acetate (3.7 mg, 16 μmol) in DMF (8 ml) and MOH (2 ml) was heated to 120° C. for 2 h under an atmosphere of carbon monoxide. After cooling to room temperature, the mixture was partitioned between water and EA. The aqueous phase was extracted with EA. The combined organic layers were dried over sodium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography (EA/HEP). 30 mg of the title compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08211885B2 |
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| Source dataset | uspto-grants-2012_07 |
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| ORD ID | ord-037cc4f5cb0549d9bae69eff9d4cf20c |
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| Source note | uspto-grants-2012_07 |
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