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5-Bromonicotinamide → 5-Bromonicotinonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Bromonicotinamide | HCID 1808 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | 5-Bromonicotinonitrile | HCID 736793 | 82% |
反応手順
Phosphorus oxychloride (5 ml) was added to 5-bromonicotinamide (2 g, 10 mmol, Avocado Research Chemicals, Ltd.) and the mixture was heated to gentle reflux for 3 hours. The mixture was allowed to cool to room temperature, poured onto ice (100 g) and extracted with ethyl acetate (3×100 mL). The combined extracts were washed successively with aqueous ammonium hydroxide and water, dried (MgSO4), filtered and the filtrate concentrated under reduced pressure. The residue was purified by chromatography (SiO2, ethyl acetate:hexanes, 1:1) to provide the title compound (1.5 g, 82% yield). MS (DCI/NH3) m/z 184 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06809105B2 |
| 出典データセット | uspto-grants-2004_10 |
| ORD ID | ord-5ed26cd2492b48b394801e0e509cf8f4 |
| 出典メモ | uspto-grants-2004_10 |