関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | 4-Chloro-2-nitro-5-(trifluoromethyl)aniline | HCID 2737645 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Chloro-5-(trifluoromethyl)benzene-1,2-diamine | HCID 2773497 | 71% |
反応手順
To a stirred mixture of 3-amino-6-chloro-4-nitrobenzotrifluoride (300 mg, 1.25 mmol) in ethanol (5 mL) was added SnCl2.2 H2O (1.40 g, 6.20 mmol) in one portion. The mixture was refluxed at 80° C. (oil bath, 90° C.) for 1 h and the solution was cooled to room temperature and ice water (20 g) was added. It was adjusted to pH=7 and extracted with ethyl acetate. The extract was dried over Mg2SO4 and evaporated to give 185 mg (71%) of 3,4-diamino-6-chlorobenzotrifluoride as a brown solid. 1H NMR (CDCl3): δ 3.404 (s, 2H); 3.717 (s, 2H); 6.754 (s, 1H); 6.974 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05620979 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-f868b29587a64c158f258690e36c6f9f |
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| 出典メモ | uspto-grants-1997_04 |
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