HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
alpha-Chloro-o-xylene → 1-(o-Methylbenzyl)-imidazole-4,5-dinitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | alpha-Chloro-o-xylene | HCID 11093 | — |
| Edukt | 4,5-Dicyanoimidazole | HCID 70729 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 1-(o-Methylbenzyl)-imidazole-4,5-dinitrile | HCID 20031024 | — |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04851424 |
| Quelldatensatz | uspto-grants-1989_07 |
| ORD ID | ord-91f2bdda383f438383e49f6107c71af1 |
| Quellennotiz | uspto-grants-1989_07 |