- AMINATION AND HYDROXYLATION OF ARYLMETAL COMPOUNDS
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In one aspect, the present disclosure provides methods of preparing a primary or secondary amine and hydroxylated aromatic compounds. In some embodiments, the aromatic compound may be unsubstituted, substituted, or contain one or more heteroatoms within the rings of the aromatic compound. The methods described herein may be carried out without the need for transition metal catalysts or harsh reaction conditions.
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Paragraph 0257
(2018/03/25)
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- Non-deprotonative primary and secondary amination of (hetero)arylmetals
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Herein we disclose a novel method for the facile transfer of primary (-NH2) and secondary amino groups (-NHR) to heteroaryl-as well as arylcuprates at low temperature without the need for precious metal catalysts, ligands, excess reagents, protecting and/or Erecting groups. This one-pot transformation allows unprecedented functional group tolerance and it is wellsuited for the amination of electron-rich, electron-deficient as well as structurally complex (hetero)arylmetals. In some of the cases, only catalytic amounts of a copper (l) salt is required.
- Zhou, Zhe,Ma, Zhiwei,Behnke, Nicole Erin,Gao, Hongyin,Kürti, László
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supporting information
p. 115 - 118
(2017/05/16)
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- Synthesis of 2-fluoro-5-polybromide method of terephthalic acid
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The invention discloses a method for synthesizing 2-fluoro-5-bromoterephthalic acid, which comprises the following steps: dissolving 2,5-dichlorobenzonitrile and dry potassium fluoride in sulfolane, and heating to react to obtain 2,5-difluorobenzonitrile (the purity is 99%); adding a new sulfolane solution, and introducing chlorine for 2 hours to obtain 6-amino-2-fluorobenzonitrile; carrying out diazotization treatment, adding acrylonitrile and hydrobromic acid, heating to react, and extracting with ethyl acetate for dilution to obtain 2-fluoro-5-bromo-p-benzonitrile; and finally, carrying out hydrolysis on the 2-fluoro-5-bromo-p-benzonitrile in a dilute sulfuric acid water solution for 8 hours, and extracting with ethyl acetate to obtain 15.44g of 2-fluoro-5-bromoterephthalic acid, wherein the yield is 83.99% above.
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Paragraph 0016; 0017
(2017/04/26)
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- Preparation of fluorinated anilines
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Fluorinated anilines, especially p-fluoroaniline and 2,4-difluoroaniline, are prepared by treating aromatic azides with anhydrous hydrogen fluoride. The aromatic azides, in turn, are prepared from the corresponding anilines by treatment with nitrous acid or salt thereof and an alkali metal azide in the presence of a mineral acid, and in an aqueous-nonaqueous, two-phase environment.
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