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2-氯-1-碘-4-硝基苯 → 2-氯-4-硝基三氟甲苯
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 2-氯-1-碘-4-硝基苯 | HCID 96640 | — |
| 反应物 | 氟化钾 | HCID 522689 | — |
| 反应物 | (三氟甲基)三甲基硅烷 | HCID 552549 | — |
| 催化剂 | 碘化亚铜 | HCID 24350 | — |
| 溶剂 | 乙醚 | HCID 3283 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | 2-氯-4-硝基三氟甲苯 | HCID 2778985 | — |
反应步骤
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.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US06462055B2 |
| 来源数据集 | uspto-grants-2002_10 |
| ORD ID | ord-add1e1d00c144897a5628bc7daef91ff |
| 来源说明 | uspto-grants-2002_10 |