2-氯-1-碘-4-硝基苯 → 2-氯-4-硝基三氟甲苯

HRID 1268021

反应方程式

HRID 1268021 反应方程式
[Cl:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1I.C[Si](C)(C)[C:14]([F:17])([F:16])[F:15].[F-].[K+]>CN(C)C=O.C(OCC)C.[Cu]I>[Cl:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[C:14]([F:17])([F:16])[F:15]

参与物

7

反应物 3

HCID 966402-氯-1-碘-4-硝基苯HCID 522689氟化钾HCID 552549(三氟甲基)三甲基硅烷

产物 1

HCID 27789852-氯-4-硝基三氟甲苯

试剂、催化剂与溶剂 3

HCID 24350碘化亚铜催化剂HCID 3283乙醚溶剂HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

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.

后处理

  1. temperatureThe solution is then cooled
  2. filtrationfiltered through diatomaceous earth
  3. washthe filtrate is washed successively with water, saturated aqueous sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent is removed under reduced pressure
  6. customthe residue is chromatographed over silica gel (1% diethyl ether in hexanes

来源与证据

ORD记录
ord-d58d2e2b8ba2456da8b56287be431750
来源数据集
uspto-grants-2003_04
专利号
US06555561B2

关联笔记

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