- The Pd-catalyzed synthesis of difluoroethyl and difluorovinyl compounds with a chlorodifluoroethyl iodonium salt (CDFI)
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Herein, we report a simple and efficient method for the direct installation of chlorodifluoroethyl group onto aromatic molecules of various aromatic amides with a new 2-chloro,2,2-difluoroethyl(mesityl)iodonium salt (CDFI). Moreover, the chlorodifluoroeth
- Niu, Yaru,Cao, Chengyao Kimmy,Ge, Chenxin,Qu, Hongmei,Chen, Chao
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supporting information
p. 1541 - 1544
(2021/10/01)
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- Preparation method of 1, 1-difluoro-2-vinyl iodide
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The invention discloses a preparation method of 1, 1-difluoro-2-vinyl iodide. The method comprises the following steps: (1) simultaneously introducing vinylidene fluoride and chlorine into a tubular reactor for reacting, condensing, and collecting the reaction product to obtain 1, 2-dichloro-1, 1-difluoroethane; (2) reacting the 1, 2-dichloro-1, 1-difluoroethane with KI in a solvent, after the reaction is finished, performing cooling, and discharging, drying the reaction liquid by distillation, and rectifying the obtained distilled liquid to obtain 1-chloro-1, 1-difluoro-2-iodoethane; and (3) reacting the obtained 1-chloro-1, 1-difluoro-2-iodoethane under the action of a magnetic catalyst, cooling and discharging after the reaction is finished, placing the reaction liquid in an external magnetic field to separate the catalyst, and rectifying to obtain the 1, 1-difluoro-2-ethylene iodide product. The method has the advantages of simple process, easily available raw materials, high yield and environmental protection.
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Paragraph 0048-0049; 0051-0052
(2021/08/28)
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- Synthesis method of 1, 1-difluoro-2-iodoethylene
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The invention discloses a synthesis method of 1, 1-difluoro-2-iodoethylene, which comprises the following steps of: (1) reacting vinylidene fluoride with iodine monochloride in a molar ratio of (1-10): 1 at 10-100 DEG C for 5-15 hours to obtain a reaction solution, adding an alkali solution and a reducing solution into the reaction solution while stirring to obtain a mixed solution, standing the obtained mixed solution for layering, and separating out a lower organic phase, carrying out rectification and purification to obtain 1-chloro-1, 1-difluoro-2-iodoethane; and (2) under the action of acatalyst, carrying out a gas-phase cracking reaction on the 1-chloro-1, 1-difluoro-2-iodoethane obtained in the step (1), and washing and drying the obtained reaction product to obtain the 1, 1-difluoro-2-iodoethylene product. The method has the advantages of simple operation, high yield and less three wastes.
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Paragraph 0031-0054
(2020/12/31)
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- Aryl difluorochloroethyl high valence iodine compound and preparation and application thereof
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The invention discloses an aryl difluorochloroethyl high-valent iodine compound and preparation and application thereof. The compound is an efficient difluorochloroethylation reagent, and a preparation method of the compound is simultaneously provided. Fi
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Paragraph 0038; 0039; 0044; 0045; 0049; 0050; 0055; 0056
(2019/10/01)
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- Radical addition of iodine monochloride to vinylidene fluoride
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The radical addition of iodine monochloride to 1,1-difluoroethylene or vinylidene fluoride (VDF) leading to a ClCF2CH2I (I)/ClCH2CF2I (II) mixture is described. Four different ways of initiation (thermal, photochemical, presence of radical initiators or redox catalysts) were used and all of them led to a high amount (≥98%) of isomer (I). The percentages of (I) and (II) isomers were determined by 19F NMR and they were also deduced from those of ClCF2CH3 and ClCH2CF2H obtained by selective reduction of the iodine atom of the product mixture, by tributylstannane. The reactivity of ICl to VDF and the high proportion of isomer (I) were interpreted by means of a thermodynamical approach from the enthalpy of formation of (I) and (II), respectively, determined by semi-empirical computations. In addition, heats of formation of both isomers and interactions between the SOMO of radicals and the HOMO of the fluoroolefin show that the mechanism of such a reaction occurs via the addition of I· to the less fluorinated side of VDF.
- Kharroubi,Manséri,Améduri,Boutevin
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p. 145 - 153
(2007/10/03)
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