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Glyoxal → Quinoxaline, 6-nitro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Glyoxal | HCID 7860 | — |
| 反応物 | 6-Quinoxalinamine | HCID 237859 | — |
| 反応物 | 4-Nitro-1,2-phenylenediamine | HCID 5111791 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Quinoxaline, 6-nitro- | HCID 96029 | — |
反応手順
Quinoxaline-6-ylamine. To a round-bottomed flask equipped with magnetic stirring was added 4-nitro-1,2-phenylenediamine (1.0 g, 6.5 mmol, Aldrich), acetonitrile (10 mL) and glyoxal (2.2 mL, 19 mmol, 40 wt. % in water, Aldrich). The reaction mixture was allowed to stir at 50° C. for 12 h, then concentrated in vacuo to yield 1.1 g crude 6-nitro-quinoxaline. The crude product was dissolved in methanol, treated with 10% Pd/C (10 mg, Aldrich) and stirred under H2 (1 atm) at 25° C. overnight. The reaction mixture was filtered through Celite and the filtrate was concentrated in vacuo to provide the title product. MS (ESI, pos. ion) m/z: 146 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07582657B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-b7881e4a193d4b18a16b0c58fc1c307b |
| 出典メモ | uspto-grants-2009_09 |