Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 1-[2-(5-Bromopyridin-2-yloxy)ethyl]azepane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,5-Dibromopyridine | HCID 69353 | — |
| 반응물 | Hexahydro-1H-azepine-1-ethanol | HCID 88615 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-[2-(5-Bromopyridin-2-yloxy)ethyl]azepane | HCID 57934072 | 96.1% |
반응 단계
To a solution of 2-azepan-1-ylethanol (5.0 g) in N,N-dimethylformamide (100 ml) was added 60% sodium hydride (1.5 g) under a nitrogen atmosphere, the solution was stirred for 1 hour at room temperature, 2,5-dibromopyridine (7.5 g) was then added thereto followed by stirring for 4.5 hours at room temperature. Water was added thereto followed by stirring, the solution was extracted with ethyl acetate, then sequentially washed with water and brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated in vacuo. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system) to provide the title compound (9.1 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07612114B2 |
| 출처 데이터셋 | uspto-grants-2009_11 |
| ORD ID | ord-2bd26d1fa4514280a606e7e691380321 |
| 출처 메모 | uspto-grants-2009_11 |