化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2-Cyano-3-fluoropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 反応物 | Pyridine, 3-fluoro-, 1-oxide | HCID 123084 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Cyano-3-fluoropyridine | HCID 7060408 | — |
反応手順
The mixture of 3-fluoro-pyridine 1-oxide (0.99 g, 8.75 mmol), trimethylsilyl cyanide (4.80 ml, 35.0 mmol), and triethyl amine (1.84 ml, 13.2 mmol) in 100 ml of CH3CN was heated at reflux overnight. The solvents were removed, under reduced pressure and the residue was partitioned between EtOAc and saturated NaHCO3. The organic portion was separated, dried with Na2SO4, filtered, condensed, the crude compound as purified by flash column chromatography (10 to 20% of EtOAc in hexanes). The titled compound was obtained as a light yellowish solid. MS (ES+): 123.1 (M+H)+. Calc'd for C6H3FN2—122.10.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08247430B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-e568494b6bbb429ab93068d83e27aa88 |
| 出典メモ | uspto-grants-2012_08 |