- Synthesis method of 2-(2, 2-difluoroethyoxyl)-6-trifluoromethyl benzenesulfonyl chloride
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The invention discloses a synthesis method of 2-(2, 2-difluoroethyoxyl)-6-trifluoromethyl benzenesulfonyl chloride. The preparation method comprises the following steps: dissolving 2-trifluoromethyl-4-nitro-bromobenzene in sulfuric acid, adding a halogenating reagent, and reacting at 50-100 DEG C for 1-8 hours; dissolving the obtained 2-bromo-3-trifluoromethyl-5-nitro-benzene halide in a solvent, and performing reduction in a reduction system; carrying out diazotization on the obtained 3-halo-4-bromo-5-trifluoromethyl-aniline, and then carrying out decomposition on the obtained 3-halo-4-bromo-5-trifluoromethyl-aniline; carrying out Grignard reaction on the obtained 2-bromo-3-trifluoromethyl-benzene halide, and then reacting with dialkyl disulfide; carrying out etherification reaction on the obtained 2-alkylthio-3-trifluorotoluene-benzene halide and 2, 2-difluoroethanol in an organic solvent under the action of an alkali; and reacting the obtained 2-(2, 2-difluoroethoxy)-6-trifluoromethyl-phenylalkyl sulfide with chlorine gas at 10-60 DEG C for 1-5 hours. The method is short in route, mild in condition, high in yield and suitable for industrial production.
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Paragraph 0039; 0046-0048; 0058; 0065-0067
(2021/06/13)
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- An improved method for the bromination of metalated haloarenes via lithium, zinc transmetalation: A convenient synthesis of 1,2-dibromoarenes
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A facile protocol for the synthesis of 1,2-dibromoarenes is described. A standard ortho-lithiation/bromination procedure, when applied to bromoarenes, resulted in poor yields of the corresponding 1,2-dibromoarenes (13-62% yield). However, transmetalation
- Menzel, Karsten,Fisher, Ethan L.,DiMichele, Lisa,Frantz, Doug E.,Nelson, Todd D.,Kress, Michael H.
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p. 2188 - 2191
(2007/10/03)
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