関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Sulfide | HCID 14804 | — |
| 反応物 | Sulfur | HCID 5362487 | — |
| 反応物 | 2-Bromo-4-nitro-1-(propan-2-yl)benzene | HCID 21531621 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 3-Bromo-4-isopropylaniline | HCID 280799 | 103.2% |
反応手順
A solution of sodium sulphide (31.2 g, 0.24 mol) and sulphur (7.7 g, 0.24 mol) was stirred at 80° C. for 15 minutes. Isopropanol (160 g) was subsequently added and the mixture was stirred at 75° C. for a further 15 minutes and 2-bromo-1-isopropyl-4-nitrobenzene (XI) (50 g, 0.19 mol) was finally added dropwise over a period of 30 minutes. After stirring for another 5 hours, the reaction was complete. For the work-up, the isopropanol was firstly distilled off and the remaining mixture was extracted with toluene/chlorobenzene. The combined organic phases were distilled under reduced pressure. 3-Bromo-4-isopropylaniline (42 g, 91 GC-% by area, 93% of theory) was obtained as a red oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440908B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-0b8cff70b7e74cb5865e34e425b77082 |
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| 出典メモ | uspto-grants-2016_09 |
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