関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 4-Methyl-1-(4-nitrophenyl)-1H-imidazole | HCID 16005169 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(4-Methyl-1h-imidazol-1-yl)benzenamine | HCID 16005170 | 10,152.9% |
反応手順
4-(4-methyl-1H-imidazol-1-yl)nitrobenzene (22.5 g; 0.87 mmol) is dissolved in abs. ethanol (250 mL), then SnCl2.2H2O (125 g; 0.55 mol) is added portion-wise, on cooling at 0° C. The resulting mixture is stirred at r.t. for 2 hours and heated at reflux overnight. The reaction mixture is then cooled at r.t. and the pH is adjusted to 12, by adding 30% KOH (500 mL), then KOH pellets under stirring. The resulting suspension is filtered and the cake is washed with ethanol, the combined filtrate and washings are concentrated and the residue is extracted with DCM. Concentration of the combined organic extracts afforded the title product as a slight brown solid (15.3 g; 80%), m.p.: 122-125° C. C10H11N3, MW 173.22.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08633208B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-38007aa131cc43e6ac40724e0553f5da |
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| 出典メモ | uspto-grants-2014_01 |
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