関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanone, 1-(5-amino-2-nitrophenyl)- | HCID 6420386 | — |
| 反応物 | Hydrobromide monohydrate | HCID 22326455 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 生成物 | 1-(5-Bromo-2-nitrophenyl)ethanone | HCID 12224157 | 75% |
反応手順
10 mmol of 3-acetyl-4-nitro-aminobenzene as a starting material was added to 100 mL of HBr/H2O (1/2, v/v) and a sodium nitrite solution was slowly added dropwise thereto in an ice bath. The reaction mixture was stirred at 60° C. for 2 hours. When the reaction was completed, the precipitate was filtered off. The filtrate was neutralized with 1N NaOH, extracted with EtOAc, dried over anhydrous sodium sulfate, distilled under reduced pressure and purified by silica gel column chromatography (hexane/EtOAc=2/1) to obtain the desired 3-acetyl-4-nitro-bromobenzene as a yellow oil (75%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07566773B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-0a65bf957c504fd4a9138c474b2d88c4 |
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| 出典メモ | uspto-grants-2009_07 |
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