関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 3-Methyl-2-butanone | HCID 11251 | — |
| 反応物 | 1-Methyl-3,5-dinitro-1H-pyridin-2-one | HCID 3621236 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Isopropyl-5-nitropyridine | HCID 45096321 | 28.3% |
反応手順
To a solution of 1-methyl-3,5-dinitro-2-pyridone (8.0 g, 40 mmol) in methyl alcohol (20 mL) was added dropwise 3-methyl-2-butanone (5.1 mL, 48 mmol), followed by ammonia solution in methyl alcohol (10.0 g, 17%, 100 mmol). The reaction mixture was heated at 70° C. for 2.5 h under atmospheric pressure. The solvent was removed under vacuum and the residual oil was dissolved in CH2Cl2, and then filtered. The filtrate was dried over Na2SO4 and concentrated to afford 2-isopropyl-5-nitro-pyridine (1.88 g, 28%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08629162B2 |
|---|
| 出典データセット | uspto-grants-2014_01 |
|---|
| ORD ID | ord-47d1cfcfb6b1412392cd0ff331ae130d |
|---|
| 出典メモ | uspto-grants-2014_01 |
|---|
