Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,5-Dimethylphenol → 2-[2-(2,5-Dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,5-Dimethylphenol | HCID 7267 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 18-Crown-6 | HCID 28557 | — |
| 반응물 | 2-(2-Bromomethylphenyl)-2-difluoromethoxyimino-acetonitrile | HCID 54541296 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 2-[2-(2,5-Dimethylphenoxymethyl)phenyl]-2-difluoromethoxyiminoacetonitrile | HCID 54404935 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05710314 |
| 출처 데이터셋 | uspto-grants-1998_01 |
| ORD ID | ord-20a91931bec440ceaefce9191690574b |
| 출처 메모 | uspto-grants-1998_01 |