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1-Butyne → 2-(1-Butynyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Butyne | HCID 7846 | — |
| 反応物 | 2-Bromopyridine | HCID 7973 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Diethylamine | HCID 8021 | — |
| 生成物 | 2-(1-Butynyl)pyridine | HCID 21299391 | 84.3% |
反応手順
After dissolving 2-bromopyridine (50 g) in diethylamine (500 mL) and adding dichlorobis(triphenylphosphine)palladium (II) (2.2 g) and copper iodide (0.3 g), the mixture was stirred at room temperature for 4 hours while introducing 1-butyne (100 g) as a gas. After bubbling in nitrogen, extraction was performed with ethyl acetate. The insoluble portion was filtered out with celite, and then the organic layer was washed with water and brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (35 g) was obtained from the n-hexane:ethyl acetate (5:1) fraction as a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091215B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-59f92c1ad5ac44d88c3cda7c11cfe96d |
| 出典メモ | uspto-grants-2006_08 |