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114435-02-8Relevant articles and documents
Recyclable polymer-supported iodobenzene-mediated electrocatalytic fluorination in ionic liquid
Sawamura, Takahiro,Kuribayashi, Shunsuke,Inagi, Shinsuke,Fuchigami, Toshio
, p. 2757 - 2760 (2010)
The electrochemical fluorination of organosulfur compounds in triethylamine/hydrofluoric acid (Et3N-5HF) with polystyrene-supported iodobenzene (PSIB) and tetraethylammonium chloride (Et4NCl) was performed successfully in an undivided cell under constant current conditions to afford the corresponding fluorinated compounds in moderate to good yields. Recycle use of the PSIB could be achieved due to its easy separation. Notably, the mediatory activity of the iodobenzene derivative was not appreciably changed even after 10 recycle uses.
Highly selective anodic monofluorination of 4-arylthio-1,3-dioxolan-2-ones: A marked solvent effect on product selectivity
Ishii,Yamada,Fuchigami
, p. 1617 - 1618 (2000)
This is the first example of a solvent effect on fluorinated product selectivity; anodic fluorination of 4-arylthio-1,3-dioxolan-2-ones in CH2Cl2 containing a fluoride supporting electrolyte using an undivided cell provided the fluoro-desulfurization product, 4-fluoro-1,3-dioxolan-2-one preferentially while anodic fluorination in DME resulted in α-fluorination, without desulfurization, selectively.
Electroorganic synthesis under solvent-free conditions. Highly regioselective anodic monofluorination of cyclic ethers, lactones, and a cyclic carbonate
Hasegawa, Masaru,Ishii, Hideki,Fuchigami, Toshio
, p. 1503 - 1505 (2002)
Regioselective anodic fluorination of cyclic ethers, lactones, and a cyclic carbonate in Et4NF·nHF (n = 4, 5) and Et3N·5HF without a solvent was successfully carried out to give the corresponding monofluorinated products in moderate yields. This is the first report of direct electrochemical fluorination of cyclic ethers, lactones, and a cyclic carbonate using anodic fluorination.
Highly Robust {Ln4}-Organic Frameworks (Ln = Ho, Yb) for Excellent Catalytic Performance on Cycloaddition Reaction of Epoxides with CO2 and Knoevenagel Condensation
Chen, Hongtai,Li, Qiaoling,Liu, Shurong,Lv, Hongxiao,Zhang, Tao,Zhang, Xiutang
, p. 14916 - 14925 (2021/12/09)
Due to the high electron charge, large ion radius, and plentiful outer hybrid orbitals of LnIII cations, microporous Ln-MOFs can be used as Lewis acidic catalysts with high catalytic activity for a variety of organic reactions, which prompts us to explore cluster-based nanoporous Ln-MOFs by employing structure-oriented ligands. Herein, the exquisite combination of coplanar [Ln4(μ3–OH)2(μ2–HCO2)(H2O)2] clusters (abbreviated as {Ln4}) and the structure-oriented multifunctional ligand of 2,6-bis(2,4- dicarboxylphenyl)-4-(4-carboxylphenyl)pyridine (H5BDCP) led to two isomorphic nanoporous frameworks of {(Me2NH2)[Yb4(BDCP)2(μ3–OH)2(μ2–HCO2)(H2O)2]·5DMF·H2O}n (NUC-38Yb) and {(Me2NH2)[Ho4(BDCP)2(μ3–OH)2(μ2– HCO2)(H2O)2]·6DMF·3H2O}n (NUC-38Ho). To the best of our knowledge, NUC-38Ho and NUC-38Yb are rarely reported {Ln4}-based three-dimensional (3D) frameworks with embedded hierarchical triangular-microporous and hexagonal-nanoporous channels, which are shaped by six rows of coplanar {Ln4} clusters and characterized by plentiful coexisting Lewis acid–base sites on the inner wall including open LnIII sites, Npyridine atoms, μ3–OH, and μ2–HCO2. Catalytic experiments performed using NUC-38Yb as the representative exhibited that NUC-38Yb possessed a high catalytic activity on the cycloaddition reactions of epoxides with CO2 under mild conditions, which can be ascribed to its structural advantages including nanoscale channels, rich bifunctional active sites, large surface areas, and chemical stability. Moreover, NUC-38Yb, as a heterogeneous catalyst, could greatly accelerate the Knoevenagel condensation reactions of aldehydes and malononitrile. Hence, this work paves the way for the construction of functional Ln-cluster-based nanoporous metal–organic frameworks (MOFs) by elaborately designing functional ligands with transnormal connection modes.
Rapid continuous flow synthesis process of fluoroethylene carbonate
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Paragraph 0022-0027, (2021/11/10)
The invention discloses a rapid continuous flow synthesis process of fluoroethylene carbonate, which comprises the following steps. Step I, EC vent nitrogen is added to the reaction kettle to be heated to the reaction temperature, thionyl chloride is added dropwise, and then an amount of AIBN is dropwise added, and the reaction 1.5 - 2h is carried out under 200 - 220Pa under reduced pressure. Step II. When the whole reaction of chloroethylene carbonate is completed, the reaction process is monitored by gas chromatography, and the reaction progress is monitored 1 - 3h through gas chromatography, and then the reaction process is monitored by gas chromatography, and the filtrate is filtered and the filtrate is filtered and the filtrate is 30 °C evaporated off under reduced pressure. The method avoids tedious work of repeated long-time operation in the past process, reduces labor intensity, shortens reaction time, and is suitable for continuous industrial production.
Preparation method of fluoroethylene carbonate
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Paragraph 0026; 0029-0031; 0034-0036; 0039-0041; ..., (2021/07/21)
The invention discloses a preparation method of fluoroethylene carbonate. The preparation method comprises the steps of preparation of phenyl iodine difluoride and preparation of fluoroethylene carbonate. The method has the beneficial effects that the synthesis of the fluoroethylene carbonate does not need to use a toxic chlorination reagent, and the cheap raw materials hydrogen peroxide and hydrogen fluoride are used; according to the preparation method, the high-purity fluoroethylene carbonate is obtained by directly distilling in a fluoroethylene carbonate synthesis reaction kettle, and the operation is simple; wherein, the acetic acid, iodobenzene, the organic solvent and the catalyst palladium acetate (II) in the preparation process of fluoroethylene carbonate are recycled, so that the cost is saved.
Fluoroethylene carbonate production method
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Paragraph 0020-0047, (2020/03/09)
The invention relates to a fluoroethylene carbonate production method. A purpose of the invention is mainly to solve the problems of high catalyst cost and low product yield in the prior art. According to the technical scheme of the invention, the method comprises: adding chloroethylene carbonate into a reactor, adding a polar aprotic solvent, a catalyst and a fluorinating reagent, reacting undera certain reaction condition, and separating reaction liquid by using a separation unit after the reaction is finished so as to obtain the fluoroethylene carbonate product. With the technical scheme of the invention, the problems in the prior art are well solved. The method of the invention can be applied to production of fluoroethylene carbonate.
Process for fluorinating inorganic or organic compounds by direct fluorination
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Paragraph 00273-00274; 0283-0286, (2020/07/14)
The invention relates to the use of a fluorinated gas, wherein the elemental fluorine (F2) is present at a high concentration, the present invention relates to a process for producing fluorinated compounds by direct fluorination using a fluorination gas in which elemental fluorine (F2) is present at a high concentration, such as a concentration of elemental fluorine (F2), in particular equal to much higher than 15 vol% or even 20 vol% (i.e., at least 15 vol% or even 20 vol%), and to a process for producing fluorinated compounds by direct fluorination using a fluorination gas. The process of the present invention relates to the manufacture of fluorinated compounds other than fluorinated benzene by direct fluorination, in particular to the preparation of fluorinated organic compounds, end products and intermediates for use in agricultural, pharmaceutical, electronic, catalyst, solvent and other functional chemical applications. The fluorination process of the invention can be carried outin batches or in a continuous manner. If the process of the invention is carried out in batches, a column (tower) reactor may be used. If the process of the invention is continuous, a microreactor may be used.
Preparation method of fluoroethylene carbonate
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Paragraph 0020; 0024; 0025, (2018/06/15)
The invention relates to a direct fluorination synthesis method of fluoroethylene carbonate, which includes steps of performing direct fluorination to ethylene carbonate and a fluorination reagent inthe presence/absence of a solvent and in the absence of a catalyst to prepare the fluoroethylene carbonate, performing fluorination regeneration to a product of the fluorination reagent after reaction, thus recycling the fluorination reagent for the direct fluorination of the ethylene carbonate. Being different from indirect fluorination, the method can efficiently produce the fluoroethylene carbonate through a direct one-step reaction, thus reducing reaction process. The product can reach high level in purity, chromaticity and yield of the product. The method is suitable for large-scale production.
Method for preparing fluoroethylene carbonate by direct fluorination
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Paragraph 0021-0023; 0025; 0027-0029, (2018/07/28)
The invention relates to a method for preparing fluoroethylene carbonate by direct fluorination. The method comprises the following steps: carrying out a reaction on fluorine gas with a fluorinating agent precursor to prepare a fluorinating agent, and directly fluorinating ethylene carbonate with the prepared fluorinating agent under a condition with a solvent or without a solvent, and without a catalyst to prepare the fluoroethylene carbonate, wherein a product obtained after the reaction of the fluorinating agent is subjected to fluorinating regeneration, and is recycled for a fluorination reaction of ethylene carbonate. According to the method provided by the invention, the problem of excessive fluorine gas activity is overcome, the fluorine gas is indirectly converted into the mild andefficient fluorinating reagent, the utilization rate and the safety of the fluorine gas are improved, and the environmental pollution is reduced.
