HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2,5-Dimethylphenol → 2-[2-(2,5-Dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2,5-Dimethylphenol | HCID 7267 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 18-Crown-6 | HCID 28557 | — |
| Edukt | 2-(2-Bromomethylphenyl)-2-difluoromethoxyimino-acetonitrile | HCID 54541296 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 2-[2-(2,5-Dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile | HCID 54404935 | — |
Reaktionsschritte
A mixture of 7.0 g of 2-(2-bromomethylphenyl)-2-difluoromethoxyimino-acetonitrile, 5.4 g of 2,5-dimethylphenol, 16.1 g of pulverized potash and 0.38 g of 18-crown-6 in 35 ml of acetonitrile is stirred at room temperature for 24 hours. For working up, water is added and exhaustive extraction with ethyl acetate is carried out. The combined organic phases are washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated by evaporation. Chromatography on silica gel with hexane/ethyl acetate (9:1) yields 2-[2-(2,5-dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile in the form of a sticky crystalline mass which, when treated with hexane, yields a fine crystal powder of m.p. 104°-108° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05710314 |
| Quelldatensatz | uspto-grants-1998_01 |
| ORD ID | ord-20a91931bec440ceaefce9191690574b |
| Quellennotiz | uspto-grants-1998_01 |