関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Styrene | HCID 7501 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 2-Bromo-4-chloroanisole | HCID 521935 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-Chloro-2-methoxy-beta-phenylstyrene | HCID 68578765 | 35.6% |
反応手順
Palladium acetate (21 mg, 7 mol %) was added to a solution of 2-bromo-4-chloroanisole (300 mg, 1.4 mmol), styrene (211 mg, 2 mmol), triethylamine (13 μL, 0.1 mmol) and triphenylphosphine (50 mg, 1.9 mmol) in acetonitrile (6 mL), and the mixture was refluxed for 8 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, the solvent was concentrated under reduced pressure and the obtained residue was diluted with ethyl acetate (15 mL). After the solution was washed successively with 2N hydrochloric acid, water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=10:1) to give the title compound (118 mg, 35.6%) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07700655B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-bc323d90db4149c59ce4603da76843ae |
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| 出典メモ | uspto-grants-2010_04 |
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