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Butanedione → 5-Bromo-8-(3,5-dimethoxy-phenyl)-2,3-dimethyl-quinoxaline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butanedione | HCID 650 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 4-Bromo-3',6-dimethoxy-biphenyl-2,3-diamine | HCID 86762042 | — |
| 生成物 | 5-Bromo-8-(3,5-dimethoxy-phenyl)-2,3-dimethyl-quinoxaline | HCID 66914591 | — |
反応手順
A mixture of 4-bromo-3′,6-dimethoxy-biphenyl-2,3-diamine (Step 85.7) (3 g, 9.3 mmol) and 2,3-butanedione (1 mL, 11.1 mmol, 1.2 equiv) in EtOH (60 mL) was stirred at reflux for 2 h, allowed to cool to it and stirred for 16 h. Additional 2,3-butanedione (0.4 ml) was added. The reaction mixture was stirred at reflux for 2 h, allowed to cool and concentrated to half of the initial volume. The resulting yellow precipitate was collected vacuum filtration providing 2.9 g of the title compound: ES-MS: 373.1/375.0 [M+H]+; tR=5.60 min (System 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536175B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-3f51cbaa30104534bbb4b36298144c4b |
| 出典メモ | uspto-grants-2013_09 |