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Ammonia → 2-Bromo-4,6-dinitroaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,4-Dinitroaniline | HCID 7321 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Bromo-4,6-dinitroaniline | HCID 15752 | 84% |
反応手順
To a stirred mixture of water (3.75 L) and acetic acid (375 mL) at rt was added 2,4-dinitroaniline (500 g, 2.73 mol) followed by dropwise addition of bromine (210 mL, 4.09 mol) over 30 min. The reaction mixture was stirred at rt for 15 min then heated to 100° C. for 2 h. The reaction mixture was then cooled to rt poured onto ice-cold water (5-6 L) and basified (pH 8-10) with aqueous ammonia. The solid thus obtained was filtered, washed with cold water and dried under vacuum. The resulting solid was washed with n-pentane to give the desired product (600 g, 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181234B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-0bbc4b2c48de4f10b61d6400c7c470a2 |
| 出典メモ | uspto-grants-2015_11 |