化工社化工社 化学情報印刷レポート · 研究参考用
Ammonia → 5,6,7,8-Tetrahydro-7-methyl-3-nitro-quinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 3-Methylcyclohexanone | HCID 11567 | — |
| 反応物 | 1-Methyl-3,5-dinitro-1H-pyridin-2-one | HCID 3621236 | — |
| 生成物 | 5,6,7,8-Tetrahydro-7-methyl-3-nitro-quinoline | HCID 23499219 | 63% |
反応手順
3-Methylcyclohexanone (0.56 g, 4.99 mmol) was mixed with 1-methyl-3,5-dinitro-2-pyridone (1.00 g, 5.02 mmol) in 1M methanolic ammonia (50 mL, 50 mmol) and heated at reflux overnight. The solvent was evaporated off and the residue was suspended in CHCl3 and flash chromatographed over silica gel (43 g) eluting with EtOAc/hexane (1:10) to afford a white solid (515 mg, 63% yield): mp 55°-56° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05866579 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-13de913f451144cd924cfe70ddbe691b |
| 出典メモ | uspto-grants-1999_02 |