関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium hydrosulfide | HCID 28015 | — |
| 反応物 | 1-Bromo-3,5-dinitrobenzene | HCID 44534 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | ar-Bromo-ar-nitrobenzenamine | HCID 44535 | 100% |
反応手順
1-Bromo-3,5-dinitrobenzene (14.77 g, 59.8 mmol) was dissolved in methanol (150 mL) and toluene (374 mL) and a solution of sodium hydrosulfide (10.06 g, 179 mmol) in water (10 mL) and methanol (150 mL) was added dropwise over a period of 60 minutes. The reaction was stirred at 80° C. for 3 hours. The reaction mixture was cooled to room temperature and then extracted 3 times with ethyl acetate. The organic layers were combined, washed with brine, dried with MgSO4, filtered, and concentrated under reduced pressure. The crude material required no further purification to yield 12.93 g (59.6 mmol, 100%) of 3-bromo-5-nitroaniline.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08735417B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-3bf75b8c14cb4c5786aaf046bf502f5c |
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| 出典メモ | uspto-grants-2014_05 |
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