化工社化工社 化学情報印刷レポート · 研究参考用
3-Methoxybenzene-1,2-diamine → 5-Methoxyquinoxaline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Methoxybenzene-1,2-diamine | HCID 184268 | — |
| 反応物 | Glyoxal-sodium bisulfite hydrate | HCID 23685989 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Methoxyquinoxaline | HCID 13238392 | 77.9% |
反応手順
Glyoxal sodium bisulphite hydrate (10.0 g) in water (80 ml) was warmed to 60° C. then a solution of 2,3-diaminoanisole (3.40 g) in ethanol (40 ml) was added. The stirred mixture was then heated to 80° C. for 1 h before addition of concentrated hydrochloric acid (6 drops). Heating was continued for 1 h. It was allowed to cool overnight, concentrated in vacuo and poured into aqueous potassium carbonate (40 ml). Ethyl acetate (3×100 ml) extracts were washed with water (100 ml) and saturated brine (50 ml) then dried over anhydrous magnesium sulphate, filtered and evaporated in vacuo to afford the title compound as a yellow solid (3.07 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06353010B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-a693d42e681d4e4b8ec4f4f16a2ddd56 |
| 出典メモ | uspto-grants-2002_03 |