Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Chloro-1-iodo-4-nitrobenzene → 2-Chloro-4-nitrobenzotrifluoride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Chloro-1-iodo-4-nitrobenzene | HCID 96640 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | (Trifluoromethyl)trimethylsilane | HCID 552549 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Chloro-4-nitrobenzotrifluoride | HCID 2778985 | — |
반응 단계
A solution of 3-chloro-4-iodo-nitrobenzene (2.26 g), trimethyl(trifluoromethyl)silane (5.68 g), copper(I) iodide (2.28 g), and potassium fluoride (0.56 g) in N,N-dimethylformamide (8 mL) is heated in a sealed tube to 80° C. for 40 hours. The solution is then cooled, diluted with diethyl ether, filtered through diatomaceous earth, and the filtrate is washed successively with water, saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure and the residue is chromatographed over silica gel (1% diethyl ether in hexanes followed by 10% ethyl acetate in hexanes is used as the eluant) to provided the desired product as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06555561B2 |
| 출처 데이터셋 | uspto-grants-2003_04 |
| ORD ID | ord-d58d2e2b8ba2456da8b56287be431750 |
| 출처 메모 | uspto-grants-2003_04 |