773-82-0Relevant articles and documents
Preparation method of fluorine-containing aryl compound
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Paragraph 0143-0150, (2021/06/12)
The invention relates to the field of organic synthesis, and especially relates to a preparation method of a fluorine-containing aryl compound. The invention provides a preparation method of a compound as shown in a formula 1. The preparation method comprises the following steps: fluorination reaction: reacting a compound as shown in a formula 2 with alkali metal fluoride in the presence of a phase transfer catalyst to prepare the compound as shown in the formula 1. According to the preparation method of the fluorine-containing aryl compound provided by the invention, a reaction system does not contain a solvent, the boiling point of the phase transfer catalyst is relatively high, solvent interference is avoided during rectification or short steaming after the reaction is finished, the distillation yield is high, and the product purity is good.
Mechanistic Insights into C(sp2)?C(sp)N Reductive Elimination from Gold(III) Cyanide Complexes
Genoux, Alexandre,González, Jorge A.,Merino, Estíbaliz,Nevado, Cristina
, p. 17881 - 17886 (2020/08/19)
A new family of phosphine-ligated dicyanoarylgold(III) complexes has been prepared and their reactivity towards reductive elimination has been studied in detail. Both, a highly positive entropy of activation and a primary 12/13C KIE suggest a late concerted transition state while Hammett analysis and DFT calculations indicate that the process is asynchronous. As a result, a distinct mechanism involving an asynchronous concerted reductive elimination for the overall C(sp2)?C(sp)N bond forming reaction is characterized herein, for the first time, complementing previous studies reported for C(sp3)?C(sp3), C(sp2)?C(sp2), and C(sp3)?C(sp2) bond formation processes taking place on gold(III) species.
Preparation method of pentafluorobenzonitrile
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Paragraph 0042; 0043; 0044; 0045; 0046; 0047; 0048; 0049, (2017/07/19)
The invention discloses a preparation method of pentafluorobenzonitrile. The method comprises the following steps: (1) introducing oxygen gas and ammonia gas into a mixed system of 2,6-dichloro-3-fluoroacetophenone, copper salt, a phase transfer catalyst and a solvent A to perform reaction to obtain 2,6-dichloro-3-fluorobenzonitrile; (2) perchlorinating the 2,6-dichloro-3-fluorobenzonitrile under the action of a catalyst to obtain 2,3,4,6-tetrachloro-5- fluorobenzonitrile; (3) adding the 2,3,4,6-tetrachloro-5-fluorobenzonitrile, KF and the phase transfer catalyst into a solvent B, and performing fluoridation to obtain the pentafluorobenzonitrile. The 2,6-dichloro-3-fluoroacetophenone used in the preparation method is a by-product in producing 2,4-dichloro-5-fluoroacetophenone, and the total yield of a single cycle can reach 83%; the raw materials are cheap and easy to obtain, the cost is reduced, and the environment is protected; and the synthetic process is simple, the operation is convenient, the yield is relatively high, the purity is good, and the pentafluorobenzonitrile is suitable for industrial production.