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Sulfuric Acid → 6-Bromo-5,7-difluoroquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Nitrobenzene | HCID 7416 | — |
| 反応物 | 4-Bromo-3,5-difluoroaniline | HCID 2736260 | — |
| 溶媒 | Glycerol | HCID 753 | — |
| 生成物 | 6-Bromo-5,7-difluoroquinoline | HCID 45108354 | — |
反応手順
A mixture of 4-bromo-3,5-difluoro-phenylamine (6.0 g, 28.8 mmole), ferrous sulfate (1.82 g), glycerol (8.6 mL), nitrobenzene (1.79 mL) and 5.0 ml of concentrated sulfuric acid (5 mL) was heated gently. After the first vigorous reaction, the mixture was heated to reflux for five hours. Nitrobenzene was removed by distillation in vacuo. The aqueous solution was acidified with glacial acetic acid, and dark brown precipitate separated, which was purified by flash chromatography (silica gel, petroleum/ethyl acetate=12/1) to return the title compound as a white solid (3.5 g, 49.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08071581B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-1a35cf78a93446f093396b06b5071da6 |
| 出典メモ | uspto-grants-2011_12 |