化工社化工社 化学情報印刷レポート · 研究参考用
Ammonia → 5,6-Dihydro-7,7-Dimethyl-3-nitro-cyclopenta[b]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 2,2-Dimethylcyclopentanone | HCID 138286 | — |
| 反応物 | 1-Methyl-3,5-dinitro-1H-pyridin-2-one | HCID 3621236 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5,6-Dihydro-7,7-Dimethyl-3-nitro-cyclopenta[b]pyridine | HCID 23499189 | 24% |
反応手順
A mixture of 1-methyl-3,5-dinitro-2-pyridone (0.8 g, 4.0 mmol), 2,2-dimethyl-cyclopentanone (0.45 g, 4.0 mmol) and ammonia solution (2.0M) in methanol (40 mL) was refluxed overnight. The solvent was removed in vacuo and the residue was dissolved in ethyl acetate. The soluble portion was flash chromatographed over silica gel (eluent 90:10 v/v ethyl acetate-hexane) to give a yellow solid (0.183 g, 24% yield).
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-66ed24339d9542aeb83127d522d74002 |
| 出典メモ | uspto-grants-1999_02 |