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alpha-Chloro-o-xylene → 1-(o-Methylbenzyl)-imidazole-4,5-dinitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | alpha-Chloro-o-xylene | HCID 11093 | — |
| 反応物 | 4,5-Dicyanoimidazole | HCID 70729 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(o-Methylbenzyl)-imidazole-4,5-dinitrile | HCID 20031024 | — |
反応手順
3.70 g of sodium are dissolved in 375 ml of ethanol and then 14.6 g of imidazole-4,5-dinitrile and 16.5 ml of o-methylbenzyl chloride are added and the whole is heated under reflux for 8 hours. The whole is concentrated to dryness by evaporation under reduced pressure and the residue is taken up in dichloromethane, washed in succession with water and with saturated sodium chloride solution, dried over sodium sulphate and concentrated to dryness by evaporation. The crude product is purified by chromatography on silica gel with toluene/ethyl acetate (5:1) and crystallised from ethyl acetate/hexane. 1-(o-methylbenzyl)-imidazole-4,5-dinitrile having a melting point of 80°-81° is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04851424 |
| 出典データセット | uspto-grants-1989_07 |
| ORD ID | ord-91f2bdda383f438383e49f6107c71af1 |
| 出典メモ | uspto-grants-1989_07 |