Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acrylate | HCID 8821 | — |
| Reactant | Tri-o-tolylphosphine | HCID 80271 | — |
| Reactant | HCID 178522917 | HCID 178522917 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178471066 | HCID 178471066 | — |
Reaction Steps
A mixture of the title compound of Example 5 (1.05 g), triethylamine (6 mL), ethyl acrylate (0.3 mL), palladium acetate (5.1 mg) and tris(o-tolyl)phosphine (42 mg) in DMF (5 mL) is heated to 100° C. for 24 h in a pressure-safe tube. The reaction is partitioned between CH2Cl2 and water. The aqueous layer is extracted with CH2Cl2 (3×). The combined organic layers are filtered, dried over Na2SO4, filtered and condensed. The crude product is purified by trituration with hot EtOAc to yield 0.461 g of the desired product as a tan solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06093732 |
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| Source dataset | uspto-grants-2000_07 |
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| ORD ID | ord-e87433d1dec84b8fb87efb34147786ee |
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| Source note | uspto-grants-2000_07 |
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