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Ethanol → 5-Nitro-2-(2-hydroxyethylpiperazin-1-yl)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 2-Chloro-5-nitrobenzonitrile | HCID 85504 | — |
| 反応物 | 1-(Piperazin-1-yl)ethan-1-ol | HCID 17769563 | — |
| 生成物 | 5-Nitro-2-(2-hydroxyethylpiperazin-1-yl)benzonitrile | HCID 22228191 | — |
反応手順
2-Chloro-5-nitrobenzonitrile (15 g) and piperazinoethanol (16 g) were added to ethanol (100 ml) and the mixture was stirred at a refluxing temperature for 1 h. The solvent was evaporated under reduced pressure. To the residue was added aqueous sodium hydroxide solution and the mixture was extracted with chloroform. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, after which the solvent was evaporated under reduced pressure. To the residue diisopropyl ether was added to allow crystallization. The crystals were recrystallized from hydrous ethanol to give 5-nitro-2-(2-hydroxyethylpiperazin-1-yl)benzonitrile (18.7 g), melting point 100–102° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07015218B1 |
| 出典データセット | uspto-grants-2006_03 |
| ORD ID | ord-e9fb11f7b6aa4ae392142ff81f74b351 |
| 出典メモ | uspto-grants-2006_03 |