関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2,6-Dinitroaniline | HCID 69070 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Bromo-2,6-dinitroaniline | HCID 3746608 | 96.2% |
反応手順
A stirred suspension of 2,6-dinitroaniline (5 g, 27.3 mmol) in glacial acetic acid (50 mL) was added bromine (1.5 mL, 30 mmol) dropwise and heated at 120° C. for 2 h. After cooling to ambient temperature, the resultant mixture was poured into water (50 mL). The precipitate solid was collected by filtration and washed with water then dried in-vacuo. The solid was re-dissolved in EtOAC, washed with water and saturated brine. The organic layer was collected and concentrated in-vacuo to give the desired product (6.88 g, 95%). 1H NMR (300 MHz, DMSO-d6) δ ppm 8.37 (br s, 2H), 8.58 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541411B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-5dd376713d8e49fe9c13b12141dbd963 |
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| 出典メモ | uspto-grants-2013_09 |
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