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Sodium Hydroxide → (2-Amino-3-chlorophenyl)amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 3-Chloro-2-nitroaniline | HCID 101068 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (2-Amino-3-chlorophenyl)amine | HCID 3462489 | 101.7% |
反応手順
12.5 g (72.4 mmol) of 3-chloro-2-nitroaniline was dissolved in methanol (250 ml), and a solution prepared by dissolving 57.2 g (253 mmol) of tin (II) chloride dihydrate in concentrated hydrochloric acid (75 mL) was added dropwise. The reaction mixture was heated with stirring for 3 hours, and concentrated under reduced pressure. Water was added to the residue thus obtained, and the solution was alkalinized with a 25% aqueous solution of sodium hydroxide, and extracted with methylene chloride. The extracted organic layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure, to obtain 10.5 g (yield: >99%) of 3-chloro-1,2-phenylenediamine as a pale magenta-colored liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08648075B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-830a6c4297cc485a9898edc0f36e3fe1 |
| 出典メモ | uspto-grants-2014_02 |