- Preparation process of 3,5-dichloro-2-iodoanisole
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The invention relates to a preparation process of 3,5-dichloro-2-iodoanisole. The preparation process comprises the following steps: sequentially adding 3,5-dichlorophenol and an organic solvent into a container, adding alkali at low temperature, carrying out uniform stirring, then recovering the temperature of a system to room temperature, performing stirring and reacting for quantitative time, slowly adding iodine at low temperature, gradually recovering to room temperature, conducting stirring overnight, quenching a reaction with acid, adding ethyl acetate for extraction, combining organic layers to obtain an intermediate product 3,5-dichloro-2-iodophenol, sequentially adding 3,5-dichloro-2-iodophenol, alkali and an organic solvent into the container, adding a methylation reagent, carrying out stirring for a reaction overnight under the condition of nitrogen protection, pouring reaction liquid into ice water, adding an organic solvent for extraction, and finally combining organic layers to obtain the final product 3, 5-dichloro-2-iodoanisole. The method is mild in reaction conditions, low in raw material price and free of dangerous goods, and has great advantages when being put into large-batch production.
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Paragraph 0046; 0053-0057
(2021/11/06)
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- Molecular spoked wheels: Synthesis and self-assembly studies on rigid nanoscale 2D objects
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We present the efficient synthesis of a new molecular spoked-wheel structure (MSW-3). Two derivatives with diameters of approximately 4 nm have been prepared. By highlighting the importance of pseudo-high-dilution conditions during cyclization, we were able to access the compounds on a several hundred milligram scale. In addition to the standard characterization (NMR spectroscopy, MS), we describe a detailed investigation of the optical properties of the fluorescent MSWs by comparison with appropriate model chromophores. Furthermore, a comprehensive study of the structure in solution by means of light- and X-ray scattering experiments has been conducted. Scanning tunneling microscopy (STM) revealed the two-dimensional organization of the molecules on highly oriented pyrolytic graphite and emphasized the spoked-wheel structure. The diameter of these molecules measured by small-angle X-ray scattering is in very good agreement with that obtained from STM and matches the results of molecular modeling. This confirms the rigidifying effect of the spokes, which results in highly shape-persistent nanometer-sized oblate organic compounds. Copyright
- Aggarwal, A. Vikas,Jester, Stefan-S.,Taheri, Sara Mehdizadeh,Foerster, Stephan,Hoeger, Sigurd
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p. 4480 - 4495
(2013/05/23)
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- Regioselective iodination of chlorinated aromatic compounds using silver salts
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The iodination of chlorinated aromatic compounds using Ag 2SO4/I2, AgSbF6/I2, AgBF4/I2, and AgPF6/I2 offers access to iodoarenes that are valuable intermediates in organic synthesis. Specifically, iodination of phenols, anisoles, and anilines with a 3,5-dichloro substitution pattern preferentially yielded the ortho, para, and para iodinated product, respectively. In the case of chlorobenzene and 3-chlorotoluene, AgSbF6/I2, AgBF4/I2, and AgPF 6/I2, but not Ag2SO4/I2, selectively introduced the iodine in para position to the chlorine substituent.
- Joshi, Sudhir N.,Vyas, Sandhya M.,Wu, Huimin,Duffel, Michael W.,Parkin, Sean,Lehmler, Hans-Joachim
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experimental part
p. 7461 - 7469
(2011/10/10)
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