関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethylsilylacetylene | HCID 66111 | — |
| 反応物 | 3-Bromo-5-nitropyridine | HCID 2762898 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 3-Nitro-5-((trimethylsilyl)ethynyl)pyridine | HCID 66715702 | 159.3% |
反応手順
To a suspension of 3-bromo-5-nitropyridine (1.0 g, 4.90 mmol), Pd(Ph3P)4 (0.57 g, 0.49 mmol), and copper iodide (0.19 g, 0.98 mmol) in triethylamine (30 mL) was added ethynyltrimethylsilane (1.0 mL, 7.35 mmol) and the reaction was purged with N2. The mixture was stirred at 80° C. for 2 h. The reaction mixture was filtered through celite and washed with ethyl acetate. The filtrate was washed with saturated solutions of NaHCO3 and NaCl. The organic layer was concentrated to afford the crude product (1.72 g) as a light brown solid: ESI MS m/z 221 [C10H12N2O2Si+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09120749B2 |
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| 出典データセット | uspto-grants-2015_09 |
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| ORD ID | ord-ca7f18693e3641b992c4d5a3cef535c2 |
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| 出典メモ | uspto-grants-2015_09 |
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