Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-Bromo-2-chloro-1-(difluoromethoxy)benzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4-Bromo-2-chlorophenol | HCID 19859 | — |
| 반응물 | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-Bromo-2-chloro-1-(difluoromethoxy)benzene | HCID 46311538 | 67.2% |
반응 단계
4-Bromo-2-chlorophenol (1.0 g, 4.8 mmol) was dissolved in DMF (35 mL) and water (5 mL) was added followed by sodium chloro(difluoro)acetate (2.0 g, 12 mmol) and cesium carbonate (3.1 g, 9.6 mmol). The mixture was stirred for 15 minutes at room temperature and then heated to 100° C. for 2 hours under nitrogen. The mixture was partitioned between water (50 mL) and TBME (50 mL). The organic phase was separated, washed brine, dried over sodium sulphate, filtered, and concentrated in vacuo. The resulting crude product was purified by silica gel chromatography eluting with 0 to 30% EtOAc in heptane to afford the title compound as colourless oil (0.83 g, 67%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09096500B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-9203e8e24d5f4596b4d18b91e4a06e90 |
| 출처 메모 | uspto-grants-2015_08 |