Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acrylate | HCID 8821 | — |
| Reactant | Tri-o-tolylphosphine | HCID 80271 | — |
| Reactant | HCID 18319552 | HCID 18319552 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 18319559 | HCID 18319559 | — |
Reaction Steps
A mixture of ethyl 2,3-dihydro-9-iodo-1-benzoxepin-4-carboxylate (0.34 g), ethyl acrylate (0.13 ml), palladium(II) acetate (2.2 mg), tri-o-tolylphosphine (6.0 mg), and triethylamine (0.15 ml) in acetonitrile (1 ml) was stirred at 100° C. under nitrogen atmosphere for 5 hours and partitioned between ethyl acetate and water. The organic layer was washed successively with water and brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was triturated in n-hexane to give a solid of ethyl 2,3-dihydro-9-[(E)-(2-ethoxycarbonylvinyl)]-1-benzoxepin-4-carboxylate (0.14 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06346527B1 |
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| Source dataset | uspto-grants-2002_02 |
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| ORD ID | ord-8ee5f0f80ee9405ba3767bf04550c424 |
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| Source note | uspto-grants-2002_02 |
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