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Aklomide → 2-Chloro-4-nitrobenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aklomide | HCID 2075 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-Chloro-4-nitrobenzonitrile | HCID 141401 | 79.7% |
反応手順
Thionyl chloride (1,000 g, 8.4 m) was then added to the 2-chloro-4-nitrobenzamide (200 g, 1 m) while the mixture was warmed. After addition, the mixture was refluxed for approximately three hours. The excess thionyl chloride was removed by distillation leaving a reaction mixture residue. Benzene (500 ml) was added to the cold reaction mixture residue to extract the reaction product. The extract was washed with diluted sodium hydroxide solution and water until neutralized and then dried over anhydrous sodium sulfate. The benzene solvent was distilled off and the reaction product was crystallized from methanol to yield 2-chloro-4-nitrobenzonitrile (145 g, 79%, mp 73°-75° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04424371 |
| 出典データセット | uspto-grants-1984_01 |
| ORD ID | ord-908ac15f209d4eec953a0050b68fc201 |
| 出典メモ | uspto-grants-1984_01 |