関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Glyoxal | HCID 7860 | — |
| 反応物 | 3-Nitro-1,2-phenylenediamine | HCID 4359525 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Quinoxaline, 5-nitro- | HCID 97512 | 97.5% |
反応手順
Oxaldehyde (40% in water; 1.43 ml, 31.3 mmol) was added to a solution of 3-nitro-o-phenylene-diamine (600 mg, 3.9 mmol) in EtOH (15 ml) and the mixture was heated at 85° C. for 2 h. The solvent was removed in vacuo, the residue was diluted in water and the aqueous phase was extracted with DCM. The organic phase was dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with DCM/MeOH (99:1) as the eluent to give the title compound (666 mg, 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09102688B2 |
|---|
| 出典データセット | uspto-grants-2015_08 |
|---|
| ORD ID | ord-aa1fa3bc74884eecb8bf344e5a373036 |
|---|
| 出典メモ | uspto-grants-2015_08 |
|---|
