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Ammonium Chloride → 3-Chloro-2,4-bis(pyridin-3-yloxy)aniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 3-Chloro-2,4-bis(pyridin-3-yloxy)-nitrobenzene | HCID 23145733 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Chloro-2,4-bis(pyridin-3-yloxy)aniline | HCID 23145696 | — |
反応手順
963 mg of ammonium chloride and 503 mg of iron powder were added to a suspension of 1.2 g of 3-chloro-2,4-bis(pyridin-3-yloxy)-nitrobenzene in 15 ml of methanol and 7.5 ml of water, and the reaction liquid was heated under reflux for 3 hours. The reaction liquid was filtered, and the solvent was evaporated away under reduced pressure. The residue was diluted with ethyl acetate, washed with water, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified with silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1 to ethyl acetate) to obtain the entitled compound as a pale yellow oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728025B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-b2bf62edf2c6442ea73ffc043f2ba1f3 |
| 出典メモ | uspto-grants-2010_06 |