Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 4-(Difluoromethoxy)benzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 4-Cyanophenol | HCID 13019 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-(Difluoromethoxy)benzonitrile | HCID 2736990 | 41% |
반응 단계
4-Cyanophenol (0.50 g, 4.2 mmol, Aldrich), sodium chlorodifluoroacetate (0.77 g, 5 mmol, Alfa Products), and sodium hydroxide (0.20 g, 5 mmol) were combined in dry DMF (2 mL) under an atmosphere of argon. After stirring at 125°-130° C. for 5 h, the mixture was cooled to RT, ethyl acetate (50 mL) was added and the organic layer was washed twice with brine. The organic extract was dried (MgSO4), filtered and evaporated. The residue was purified by flash chromatography (silica gel, 25% ethyl acetate/hexanes) to provide a white solid. The solid was sublimed (1 mm Hg, 23° C.) to provide the title compound as colorless crystals (0.29 g, 41%). mp 33°-35° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05731477 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-9878f8a1a69f4990b1191065d489c660 |
| 출처 메모 | uspto-grants-1998_03 |