関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 反応物 | Ethyl 4-vinylbenzoate | HCID 10866858 | — |
| 反応物 | 4,4-Dimethyl-7-bromo-1-phenylthio-3,4-dihydronaphthalene | HCID 15896018 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Ethyl (E)-4-[2-(5,6-dihydro-5,5-dimethyl-8-(phenylthio)naphthalenyl)ethenyl]benzoate | HCID 19695074 | — |
反応手順
To a degassed solution of 0.35 g (1.0 mmol) of 2-bromo-5,6-dihydro-5,5-dimethyl-8-(phenylthio)-naphthalene (Compound A35) and 0.34 g (1.9 mmol) of ethyl 4-vinylbenzoate in 4.0 mL of triethylamine, was added 0.066 g (0.2 mmol) of tri-o-tolylphosphine and then 0.025 g (0.1 mmol) of palladium(II) acetate. The reaction was heated at 90° C. for 2.25 h. The reaction was concentrated in vacuo. The residue was purified by flash chromatography (silica, 5% ethyl acetate in hexane), followed by recrystallization using EtOH to afford the title compound as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05723666 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-6359f090cbac49c6a126e41999e4f8b9 |
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| 出典メモ | uspto-grants-1998_03 |
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