Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 5-Bromo-3-(2,6-dimethylpyridin-3-yloxy)picolinonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,6-Dimethyl-3-pyridinol | HCID 70732 | — |
| 반응물 | 5-Bromo-3-nitropyridine-2-carbonitrile | HCID 2769698 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Bromo-3-(2,6-dimethylpyridin-3-yloxy)picolinonitrile | HCID 67486452 | 101.2% |
반응 단계
To a 0° C. solution of 2,6-dimethylpyridin-3-ol (10 g, 81.2 mmol) in DMF (50 ml) was added sodium hydride (60% dispersion in oil, 3.4 g, 85 mmol). After 15 minutes, 5-bromo-3-nitropicolinonitrile (18.5 g, 81 mmol) was added and the mixture was allowed to warm slowly to ambient temperature. The reaction mixture was slowly added to 500 mL of rapidly stirring water. A light red solid formed and then the material formed a gum. The gum was extracted into ethyl acetate, and the organics washed with brine, dried over MgSO4 and concentrated in vacuo to afford 5-bromo-3-(2,6-dimethylpyridin-3-yloxy)picolinonitrile (25 g, 82 mmol, 101% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08853409B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-d3ebc3b23e2d4d389e88503e7fd5fbc1 |
| 출처 메모 | uspto-grants-2014_10 |