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1-Chloro-2,4-Dinitrobenzene → 4-Chloro-M-phenylenediamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Chloro-2,4-Dinitrobenzene | HCID 6 | — |
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Cyanamide | HCID 9864 | — |
| 反応物 | Formamidine acetate | HCID 160693 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Chloro-M-phenylenediamine | HCID 21209 | — |
反応手順
1.5 g of cyanamide, 1.5 g of acetic acid, 2 g of Raney nickel (60%, aqueous), and 120 ml of methanol are introduced in an autoclave equipped with gas introduction stirrer. Under a hydrogen pressure of 4 bar and a temperature of 25° C., the cyanamide is hydrogenated quantitatively to the formamidine acetate. 40.8 g of 1-chloro-2,4-dinitrobenzene are then added to the autoclave, and the hydrogenation is carried out at a pressure of 10 bar and a temperature of 60° C. The hydrogenation time is 1 hour. 1-Chloro-2,4-diaminobenzene, 97.5% pure (analysed as 1-Chloro-2,4-acetamidobenzene by liquid chromatography), is obtained in quantitative yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04960936 |
| 出典データセット | uspto-grants-1990_10 |
| ORD ID | ord-854f343b508f4d689cd02c64dc88fc11 |
| 出典メモ | uspto-grants-1990_10 |