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Water → 2-Bromo-1,3-dimethyl-4-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4-Nitro-m-xylene | HCID 6991 | — |
| 反応物 | Potassium Bromate | HCID 23673461 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Bromo-1,3-dimethyl-4-nitrobenzene | HCID 12395905 | — |
反応手順
To a solution of 4-nitro-m-xylene (0.96 g, 6.4 mmol) in acetic acid (8 mL) and sulfuric acid (4 g) and Water (4 mL) was added potassium bromate (1.18 g, 7 mmol) portion-wise over 20 minutes. The mixture was allowed to stir 72 hours at room temperature. The desired product was recovered together with starting material after partition between water, and ethyl acetate (2×) washing with water, saturated sodium bicarbonate solution and brine. The organic layer was dried over sodium sulfate, decanted and upon concentration under reduced pressure yielded the desired 2-bromo-1,3-dimethyl-4-nitrobenzene and starting material as an oily solid. The crude mixture was carried on to step two without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07579340B2 |
| 出典データセット | uspto-grants-2009_08 |
| ORD ID | ord-c0c86338a88b4fbca28da25bfea9236a |
| 出典メモ | uspto-grants-2009_08 |