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Water → 2-Bromo-4-(tert-butyl)-6-nitroaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 4-tert-Butyl-2-nitroaniline | HCID 80573 | — |
| 反応物 | Pyridinium hydrobromide | HCID 21226041 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Bromo-4-(tert-butyl)-6-nitroaniline | HCID 50997856 | 94% |
反応手順
A suspension of 4-tert-butyl-2-nitroaniline (1.033 g, 5.32 mmol) in glacial acetic acid (7.8 mL) was warmed with a heat gun until all solids had dissolved. The solution was then cooled and treated portion wise with pyridinium hydrobromide perbromide (1.96 g, 6.12 mmol). After addition, the solution was stirred at room temperature for 1 h. The mixture was added to water (50 mL) and treated with a small amount of sodium sulfite. After stirring for 30 min, the precipitate was collected by filtration. The solid obtained was washed with water and dissolved in EtOAc. Washed with water and brine. Dried over Na2SO4, filtered and concentrated under vacuum to provide the title compound as a yellow-orange solid (1.36 g, 94%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09095590B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-2cbc1eeeca104231a92bd89be3d30091 |
| 出典メモ | uspto-grants-2015_08 |