関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 4-bromobenzoate | HCID 22043 | — |
| 反応物 | 1-Eth-1-ynyl-4-(pentyloxy)benzene | HCID 2775119 | — |
| 触媒 | Triphenylphosphine | HCID 11776 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Ethyl 4-(4-n-pentyloxyphenylethynyl)benzoate | HCID 22713259 | 35.2% |
反応手順
To a suspension of ethyl 4-bromobenzoate (1.37 g), (4-n-pentyloxyphenyl)acetylene (565 mg), triphenylphosphine (16 mg) and copper(I) iodide (6 mg) in triethylamine (10 ml) and pyridine (4 ml) was added palladium(II) chloride bis(triphenylphosphine) (21 mg) and the reaction mixture was stirred for 24 hours at 80° C. After cooling, the precipitate was filtered off, and the filtrate was evaporated under reduced pressure. The residue was taken up to dichloromethane, and the solution was washed successively with 1N HCl, water, brine and dried over magnesium sulfate. The solvents were removed under reduced pressure and the residue was triturated with acetonitrile, collected by filtration and dried under reduced pressure to give ethyl 4-(4-n-pentyloxyphenylethynyl)benzoate (355 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06743776B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-75df36affa3b4e1c9e154e2606ab4cdf |
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| 出典メモ | uspto-grants-2004_06 |
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