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3-Chloro-5-nitrotoluene → 3-Chloro-5-methylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Chloro-5-nitrotoluene | HCID 297887 | — |
| 反応物 | Tin dichloride-dihydrate | HCID 131729857 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 3-Chloro-5-methylaniline | HCID 12475434 | — |
反応手順
2.4 g of 3-chloro-5-nitro-toluene are dissolved in 35 ml of ethanol, combined with 15.8 g tin dichloride-dihydrate and refluxed for 3 hours. The solvent is eliminated in vacuo, the residue is taken up in 4 M sodium hydroxide solution and filtered through kieselguhr. The filter cake is washed thoroughly with ethyl acetate. The aqueous phase is extracted 3 times with ethyl acetate and the combined organic phases are washed with saturated sodium chloride solution and dried on magnesium sulphate. The solvent is eliminated in vacuo and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 81:15 to 70:30).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08232312B2 |
| 出典データセット | uspto-grants-2012_07 |
| ORD ID | ord-8ba689a804ec4c51a97fd6a969edc167 |
| 出典メモ | uspto-grants-2012_07 |