化工社化工社 化学情報印刷レポート · 研究参考用
2,5-Dimethylphenol → 2-[2-(2,5-Dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Dimethylphenol | HCID 7267 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 2-(2-Bromomethylphenyl)-2-difluoromethoxyimino-acetonitrile | HCID 54541296 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-[2-(2,5-Dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile | HCID 54404935 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05710314 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-20a91931bec440ceaefce9191690574b |
| 出典メモ | uspto-grants-1998_01 |