関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-Ethynylpyridine | HCID 642801 | — |
| 反応物 | 2-bromo-N,N-dimethylpyridin-3-amine | HCID 86643498 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Dimethyl-(2-pyridin-4-ylethynyl-pyridin-3-yl)-amine | HCID 68429284 | 45% |
反応手順
A mixture of 2 g of (2-Bromo-pyridin-3-yl)-dimethyl-amine (9.95 mmoles), 1.24 g of 4-ethynyl pyridine (12 mmoles) in 120 mL of a 1/1 mixture of triethylamine and dimethylformamide is stirred under argon at room temperature. 750 mg of bis(triphenylphosphine)palladium dichloride and 400 mg of copper iodide are added to the reaction mixture which is further stirred at room temperature for 3 hours. The reaction mixture is poured into ammonium chloride solution and extracted with ethyl acetate. The organic phase is washed with water and dried over magnesium sulfate. The solid residue after concentration is purified by chromatography on silica gel (ethylacetate/hexane 1/1) to give 1 g of Dimethyl-(2-pyridin-4-ylethynyl-pyridin-3-yl)-amine as orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08084395B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-4951c305bfd4457389ec8e82d453e684 |
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| 出典メモ | uspto-grants-2011_12 |
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