化工社化工社 化学情報印刷レポート · 研究参考用
Hydrazinium bromide → 1160227-03-1
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazinium bromide | HCID 159693 | — |
| 反応物 | 3-Oxo-2-(pyridin-3-yl)butanenitrile | HCID 67362649 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1160227-03-1 | HCID 67363636 | — |
反応手順
3-Oxo-2-pyridin-3-yl-butyronitrile (step 1) (1.00 g, 6.49 mmol) was dissolved in EtOH (10 ml) and water (2 ml). Hydrazine hydrobromide (2.82 g, 24.97 mmol) was added and the reaction mixture was heated at reflux for 1 hour. The solvent was removed in vacuo and the residue was partitioned between EtOAc and sat. NaHCO3. The organic phase was washed with water and brine, dried (MgSO4), filtered and the solvent was removed in vacuo to afford the title compound which was used without further purification; 1H NMR (d6-DMSO, 400 MHz) δ 11.51 (1H, br), 8.60 m), 8.40 (1H, m), 7.72 (1 h, m), 7.39 (1H, m), 4.60 (2H, br), 2.19 (3H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835444B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-50f9fa1b87994be683590f893a48119e |
| 出典メモ | uspto-grants-2014_09 |