Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitric Acid → 1-(2-Fluoro-5-nitrophenyl)ethan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | o-Fluoroacetophenone | HCID 96744 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 1-(2-Fluoro-5-nitrophenyl)ethan-1-one | HCID 2781067 | — |
반응 단계
In a 3-neck flask equipped with an internal thermometer was added sulfuric acid and cooled to −10° C. in an ice/salt/water batch. 2′-fluoroacetophenone(1 eq) in sulfuric acid was added dropwise over 10 minutes via addition funnel to produce a solution of 0.2M. Nitric acid (1.15 eq) in sulfuric acid was then added dropwise at a rate not to exceed 5° C. After complete addition resulting solution was allowed to stir at for 30 minutes. Solution was poured onto ice and extracted with ethyl acetate. Organics were washed with a saturated solution of sodium bicarbonate, brine, dried with sodium sulfate and concentrated. Crude product was purified using flash chromatography (85% Hex:15% EtoAc) on silica to afford 1-(2-fluoro-5-nitrophenyl)ethanone.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07423150B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-6bccb15750864f96b01b595ff9affa02 |
| 출처 메모 | uspto-grants-2008_09 |