Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Methylpyridine → 1-(4-Fluorophenyl)-2-(pyridin-4-yl)ethan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Methylpyridine | HCID 7963 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Benzoic acid, 4-fluoro-, ethyl ester | HCID 67976 | — |
| 반응물 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(4-Fluorophenyl)-2-(pyridin-4-yl)ethan-1-one | HCID 10330881 | 86.1% |
반응 단계
To a solution of 4-methylpyridine (74.4 g) and ethyl 4-fluorobenzoate (134.4 g) in dry tetrahydrofuran (600 ml) was added a 1.0M solution of lithium bis(trimethylsilyl)amide in tetrahydrofuran (1.6 l) dropwise with ice cooling. The mixture was stirred at ambient temperature for 30 minutes. To the reaction mixture was added hexane (2.2 l) and the separated solid was collected, washed with hexane and dried. The obtained solid was dissolved in 3N-hydrochloric acid (800 ml) and the solution was neutralized with an aqueous saturated sodium bicarbonate solution. The separated solid was collected, washed with water and dried to give 1-(4-fluorophenyl)-2-(pyridin-4-yl)ethan-1-one (148 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05624931 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-e20b73be0df544f7862a4b355c833ffe |
| 출처 메모 | uspto-grants-1997_04 |