関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | 4-Nitro-1,2-bis(trifluoromethyl)benzene | HCID 2736166 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3,4-Bis(trifluoromethyl)aniline | HCID 1548579 | 99.5% |
反応手順
A mixture of 261 mg (1.00 mmol) of 3,4-bis(trifluoromethyl)nitrobenzene and 989 mg (5.23 mmol) of SnCl2 in 6 mL of ethanol was heated at 70° C. for 2 h. It was evaporated to dryness and the residue was treated with 1N NaOH to pH=13. White precipitate was observed. The mixture was extracted by CHCl3 (4×8 mL). The extract was dried (MgSO4) and evaporated to leave 228 mg (99%) of oil. 1H NMR (CDCl3), 4.167 (sb, 2), 6.803 (d, 1, J=7.41), 7.026 (s, 1), 7.579 (d, 1, J=8.58). 19F NMR (CDCl3), 55.014 (q, 3), 56.919 (q, 3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05622952 |
|---|
| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-3713417fb74441f18251fa41192506d9 |
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| 出典メモ | uspto-grants-1997_04 |
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