98-46-4Relevant articles and documents
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Olah et al.
, p. 147 (1957)
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Preparation method of m-nitrobenzotrifluoride
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Paragraph 0038-0045; 0049-0051, (2020/08/22)
The invention relates to a preparation method of m-nitrobenzotrifluoride. The method includes carrying out nitration reaction on trifluorotoluene, concentrated sulfuric acid and nitric acid in an organic solvent; specifically, stirring trifluorotoluene, an organic solvent and concentrated sulfuric acid under the condition that the temperature is controlled to be 30-40 DEG C, adding fuming nitric acid is dropwise, performing a heat preservation reaction for 6-10 h; after the reaction is completed, standing and performing liquid separation, adjusting the pH of an organic phase to be alkaline with an alkaline aqueous solution, performing desolvation on the organic phase, and finally performing reduced pressure distillation to obtain m-nitrotrifluorotoluene. According to the invention, dichloroethane, carbon tetrachloride and other chlorinated non-polar solvents are used as reaction solvents for nitration reaction, so violent heat release in the nitration reaction process is reduced, the reaction conditions are mild, and the safety is improved; meanwhile, the dosage of acid and the dosage of post-treatment alkali are greatly reduced, and three wastes are reduced, so that the post-treatment is simple, the product is easy to separate, the operation is simple and convenient, side reactions are few, the yield is high, the product purity is high and the process pollution is small.
Catalytic trifluoromethylation of iodoarenes by use of 2-trifluoromethylated benzimidazoline as trifluoromethylating reagent
Akiyama, Takahiko,Ishikawa, Taisuke,Kamiyama, Nanami,Uchikura, Tatsuhiro
supporting information, p. 2442 - 2447 (2020/11/07)
The trifluoromethylation of iodoarenes was accomplished by use of a 2-trifluoromethylbenzimidazoline derivative as the trifluoromethylating reagent and a catalytic amount of Cu(I) in the presence of 2,2'-bipyridyl as the ligand. Through a mechanistic study, we found that the oxidative addition of the iodoarene to the Cu(I)–CF3 species is the rate-determining step.