2043-47-2Relevant academic research and scientific papers
New insights on the asymmetric hydroboration of perfluoroalkenes
Segarra, Anna M.,Claver, Carmen,Fernandez, Elena
, p. 464 - 465 (2004)
Enantioselective access to Markovnikov regioisomeric perfluoroalcohols is achieved in the presence of chiral cationic rhodium complexes and specific hydroborating reagents.
Environmentally friendly preparation method of fluorine-containing acrylate
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Paragraph 0019; 0022; 0029; 0032, (2019/01/06)
The invention relates to the technical field of preparation of new fluorine-containing materials, particularly to an environmentally friendly preparation method of fluorine-containing acrylate. The environmentally friendly preparation method comprises: carrying out a reaction on short-chain perfluoroiodoalkane and ethylene, separating, and purifying to obtain perfluoroalkylethyl iodide; carrying out hydrolysis on the perfluoroalkylethyl iodide, separating, and purifying to obtain perfluoroalkylethanol; and carrying out a reaction on the perfluoroalkylethanol and acrylic acid, separating, and purifying to obtain the product. According to the present invention, the perfluorooctyl-free product is synthesized, the potential risk of PFOA production cannot exist, and the obtained product is theenvironmentally friendly product, and meets the national industrial policy; the preparation method is simple, and is suitable for industrial production; and the reaction conversion rate is high, and the purity of the intermediate product is high, such that the subsequent reaction is easily performed, the yield is easily increased, and the cost is reduced.
Method for preparing perfluoroalkyl ethanol
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Paragraph 0026-0032, (2017/11/29)
The invention discloses a method for preparing perfluoroalkyl ethanol. The method comprises the following steps: enabling perfluoroalkyl ethyl iodide, a mixed solvent and water to react, and separating and purifying the obtained mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water, thereby obtaining the perfluoroalkyl ethanol product, wherein the separation and purification comprise the following steps: (1) adding a mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water into a rectifying tower for performing reduced pressure distillation, controlling the vacuum degree to be -0.91 to -0.96MPa so as to obtain distillate containing perfluoroalkyl ethanol, by-product olefins and water and bottom liquid, performing strong base treatment on the bottom liquid, and filtering to obtain the recycled mixed solvent; and (2) performing azeotropic distillation on the distillate, thereby obtaining the mixed solution of the by-product olefins and water and the product perfluoroalkyl ethanol. The method disclosed by the invention has the advantages of simplicity in process, greening, environment friendliness, convenience, high efficiency and low cost.
Synthesis of 2-(perfluoroalkyl)ethyl potassium sulfates based on perfluorinated Grignard reagents
Paterová, Jana,Skalicky, Martin,Rybá?ková, Markéta,Kví?alová, Magdalena,Cva?ka, Josef,Kví?ala, Jaroslav
experimental part, p. 1338 - 1343 (2011/02/22)
The first example of nucleophilic substitution with perfluoroalkyl Grignard reagents on the sp3 carbon centre is described. Thus, a series of organometals RF-MgBr, prepared from perfluorinated alkyl iodides RF-I with RF = C4F9, C 6F13, C8F17, C10F 21 and C12F25, reacted with 1,3,2-dioxathiolane-2,2-dioxide to afford the corresponding 2-(perfluoroalkyl) ethyl magnesium sulfates, which were isolated after metathesis to the corresponding potassium salts. In the model reaction, perfluorohexylmagnesium iodide was reacted with methyl triflate yielding polyfluorinated alkane. The attempts to extend the reaction to 1,3,2-dioxathiane-2,2-dioxide were unsuccessful due to its inferior reactivity and only reduced polyfluoroalkane and the product of coupling were detected in the reaction mixture. Polyfluorinated sulfates are easily hydrolyzed with hydrochloric or triflic acid to the corresponding alcohols, which is an alternative to standard transformation of perfluoroalkyl iodides to 2-(perfluoroalkyl)ethanols. Quantum-chemical calculations of the PES of the reaction with both sulfur-containing heterocycles found that the failure of the reaction with 1,3,2-dioxathiane-2,2-dioxide is caused by higher activation energy of the process.
Purification of fluorinated alcohols
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Page/Page column 4-5, (2008/06/13)
A process for reducing the level of perfluoroalkanoic acids, perfluoroalkanoic esters, and perfluoroalkyliodides in fluorinated alcohols comprising heating a fluorinated alcohol, or mixtures thereof, containing said acids, esters, or iodides to a temperature of at least 175° C. in the presence of water and a base additive is disclosed.
Process for producing a polyfluoroalkyl (meth)acrylate
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Page 5; 6, (2008/06/13)
A process for producing a polyfluoroalkyl (meth)acrylate, which comprises isolating, from a reaction mixture containing a polyfluoroalkyl (meth)acrylate obtained by reacting a polyfluoroalkyl iodide of the formula CnF2n+1(CH2)mI (wherein n is an integer of from 2 to 7, and m is an integer of from 1 to 4) with a metal (meth)acrylate in tert-butanol, said polyfluoroalkyl (meth)acrylate by the following steps (1) to (3):(1) a step of taking out a crude liquid from the reaction mixture by solid-liquid separation;(2) a step of distilling the crude liquid to separate it into compound group A of compounds having a lower boiling point than the polyfluoroalkyl (meth)acrylate and compound group B of the polyfluoroalkyl (meth)acrylate and compounds having a higher boiling point than the polyfluoroalkyl (meth)acrylate; and(3) a step of distilling and purifying the polyfluoroalkyl (meth)acrylate from the compound group B in the presence of a polymerization inhibitor.
Catalysts for the preparation of fluorinated alcohols and process for the preparation of fluorinated alcohols
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Page column 8-9, (2008/06/13)
The present invention provides a catalyst for preparing a fluorine-containing alcohol compound, the catalyst having at least one component selected from elements in Group 1B, Group 2B, Group 6A, Group 7A and Group 8 of the periodic table, ions of these elements, oxides containing these elements, hydroxides containing these elements and salts containing these elements, said component being supported on at least one complex oxide selected from Si—Al complex oxides, Al—P complex oxides and Si—Al—P complex oxides; and a method for preparing a fluorine-containing alcohol compound, the method comprising reacting a halogenated fluorine compound with water in the presence of the catalyst. According to the present invention, a fluorine-containing alcohol compound can be prepared at a relatively low reaction temperature and in a high yield.
Investigation of the factors controlling the regioselectivity of the hydroboration of fluoroolefins
Ramachandran, P. Veeraraghavan,Jennings, Michael P.
, p. 386 - 387 (2007/10/03)
Either Markovnikov or anti-Markovnikov regioselectivity can be achieved at will during the hydroboration-oxidation of perfluoroalkyl(aryl)ethylenes by varying the hydroborating agent.
Critical role of catalysts and boranes for controlling the regioselectivity in the rhodium-catalyzed hydroboration of fluoroolefins
Ramachandran, P. Veeraraghavan,Jennings, Michael P.,Brown, Herbert C.
, p. 1399 - 1402 (2008/02/09)
(formula presented) Catalytic hydroboration of perfluoroalkylethylenes (RFCH=CH2) with cationic and neutral rhodium complexes allows for selective access to either regioisomeric alcohol after hydroboration with catechol- and pinacolboranes, followed by oxidation with alkaline hydrogen peroxide.

