関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 1,2-Dimethoxy-4,5-dinitrobenzene | HCID 222989 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4,5-Dimethoxy-2-nitroaniline | HCID 4653152 | 119.3% |
反応手順
4.50 g (20.0 mmol) 4,5-dimethoxy-1,2-dinitrobenzene was taken into 50.0 mL EtOH/8.4 mL AcOH mixture. To this was added 4.00 g powdered iron (O). The reaction was heated to an oil bath temperature of 70° C. overnight. The reaction was allowed to cool to room temperature and was poured into 400 mL H2O. Aqueous layer was extracted several times with diethyl ether. Organic layers were dried over magnesium sulfate and evaporated under reduced pressure to give 4.73 g orange solid as a mixture of starting material and product. This solid was purified over silica gel (30% DCM in hexanes) to give the title compound 86A as an orange solid (1.15 g, 5.80 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07019147B1 |
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| 出典データセット | uspto-grants-2006_03 |
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| ORD ID | ord-f7894d8e5a5e45aa96d7481853c32e55 |
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| 出典メモ | uspto-grants-2006_03 |
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