Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 5-Fluoro-2-nitroanisole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | 5-Fluoro-2-nitrophenol | HCID 9937 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Fluoro-2-nitroanisole | HCID 2779250 | 82.7% |
반응 단계
To a solution of 4-fluoro-2-hydroxy-1-nitrobenzene (5.0 g, 31.8 mmol) in DMF (10 mL) was added K2CO3 (13.1 g, 95.4 mmol). The reaction mixture was stirred at RT for 1 h followed by addition of methyl iodide (9.93 g, 69.9 mmol) and the reaction mixture was stirred at 60° C. for 2 h. The reaction mass was concentrated and quenched in water. The reaction mass was basified with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 4.5 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 3.93 (s, 3H), 6.97 (t, J=7.8 Hz, 1H), 7.31 (d, J=8.7 Hz, 1H), 8.02 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09439890B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-e8f86d536e734cf39f9dfc110116cfd1 |
| 출처 메모 | uspto-grants-2016_09 |