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Hydrochloric Acid → 2-Chloro-5-methylbenzene-1,3-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Chloro-3,5-dinitrotoluene | HCID 78918 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Chloro-5-methylbenzene-1,3-diamine | HCID 12402979 | 70% |
反応手順
4-chloro-3,5-dinitrotoluene (9.0 gm.) is dissolved in 50% ethanol (30 ml.). Electrolytically reduced iron powder (14.2 gm.) is added and the stirred reaction mixture heated to reflux. Concentrated HCl (1 ml.) in 50 % ethanol (5 ml.) is added dropwise and refluxing continued for one hour. The reaction mixture is allowed to cool slightly and made basic (pH 8) with 20% NaOH, then the iron removed by filtration. The filtrate is taken to dryness under reduced pressure and the residue extracted with hot Skellysolve "B" (700 ml.). The product precipitates in long needles that were collected by filtration (4.57 gm., m.p. 114°-115.5°, 70% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04089973 |
| 出典データセット | uspto-grants-1978_05 |
| ORD ID | ord-d0d14ab86adc40c286ba14ab36a0453d |
| 出典メモ | uspto-grants-1978_05 |