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Water → 4-Trifluoromethyl-1,2-phenylenediamine
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 | Benzenamine, 2-nitro-4-(trifluoromethyl)- | HCID 67865 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Trifluoromethyl-1,2-phenylenediamine | HCID 520822 | 96.9% |
反応手順
A solution of 2-nitro-4-trifluoromethylaniline (5.000 g, 24.26 mmol, Aldrich, used as received) and SnCl2.2 H2O (20.00 g, 88.64 mmol, Aldrich, used as received) in absolute ethanol (50 mL) was refluxed for 45 min. It was then poured into ice (85 g) and basified with 10% aq. NaHCO3 (250 mL). The resulting suspension was extracted with ethyl acetate (400 mL). The ethyl acetate extract was dried over Na2SO4 and evaporated to give 4.14 g (87%) of pure 4-trifluoromethyl-1,2-phenylenediamine as a red powder.
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 |
| ORD ID | ord-62109381f5f14189913bf106ba37e015 |
| 出典メモ | uspto-grants-1997_04 |