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2-Chloro-1-iodo-4-nitrobenzene → 2-Chloro-4-nitrobenzotrifluoride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloro-1-iodo-4-nitrobenzene | HCID 96640 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | (Trifluoromethyl)trimethylsilane | HCID 552549 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-4-nitrobenzotrifluoride | HCID 2778985 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06555561B2 |
| 出典データセット | uspto-grants-2003_04 |
| ORD ID | ord-d58d2e2b8ba2456da8b56287be431750 |
| 出典メモ | uspto-grants-2003_04 |