- Amine-induced decomposition of perfluoroalkanesulfonyl fluorides
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Perfluoroalkanesulfonyl fluorides (CnF2n+1SO 2F) decompose slowly even at -20°C in the presence of tertiary heteroaromatic or aliphatic amines to form the corresponding perfluorinated alkanes (CnF2n+2
- Bennua-Skalmowski, Baerbel,Klar, Ulrich,Vorbrueggen, Helmut
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- SYNTHESIS OF PERFLUOROALKYL CARBOXYLIC ACIDS BY REACTION OF PERFLUOROALKYL IODIDES WITH ELECTROGENERATED SUPEROXIDE ION
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The electrogenerated superoxide ion O2 is shown to react with perfluoroalkyliodides to afford F-alkyl carboxylic acids.A mechanism is proposed on the basis of the results obtained in preparative experiments and by cyclic voltammetry.
- Amatore, C.
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- Synthesis method of straight-chain perfluoroalkanes
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The invention relates to a synthesis method of straight-chain perfluoroalkanes, which comprises the following steps: reaction of perfluoroalkyl iodine with alcohol solution of sodium alcohol at a certain temperature to purify 1-hydroperfluoroalkanes; reaction of 1-hydroperfluoroalkanes with fluorine gas at a certain temperature to purify straight-chain perfluoroalkanes. The synthesis method of theinvention has mild reaction conditions, high product yield, and is beneficial to cost saving. The process has low energy consumption, easy operation and is conducive to industrial production.
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- Production raw material of liquid ventilation fluid and material for ophthalmic surgery and continuous preparation method of production raw material
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The invention provides a production raw material of liquid ventilation fluid and a material for an ophthalmic surgery and a continuous preparation method of the production raw material. The productionraw material comprises fluorine and an octane organic matter, the molar ratio of the fluorine to the octane organic matter is 20: 1-25: 1, the fluorine is mixed gas of pure fluorine or fluorine and inert gas, and the concentration of the fluorine is not lower than 10%; and the octane organic matter is a mixture of octane, an octane homologue or a mixture of the octane organic matter and inert gas. The production raw material is suitable for being produced continuously on a large scale, reaction conditions are easy to control, the yield is high, by-products are less, reaction products are easyto separate and purify, and waste gas, waste water and solid wastes are not discharged in a production process. By the method of the invention, perfluorooctane of which the purify is greater than orequal to 99% can be prepared, and can serve as the production raw material of liquid ventilation fluid and a preparation for the ophthalmic surgery.
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Paragraph 0019-0022
(2019/01/23)
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- Preparation method for perfluoroalkane
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The invention discloses a preparation method for perfluoroalkane. The preparation method comprises the following steps: adding a fluorination reagent into a reaction vessel, stirring the fluorination reagent at room temperature, introducing fluorine-nitrogen gas mixture into the reaction vessel for activation of the fluorination reagent and continuing stirring for half an hour, wherein the concentration of fluorine gas in the fluorine-nitrogen gas mixture is 0.5 to 10%, and the molar weight of the fluorine-nitrogen gas mixture is 1 to 5% of the molar weight of the fluorination reagent; after completion of stirring, relieving residual pressure in the reaction vessel, and adding perfluoroalkyl halide and a solvent into the reaction vessel for a reaction at 150 to 200 DEG C for 5 to 10 h, wherein a mol ratio of perfluoroalkyl halide to the fluorination reagent is (1: 1) to (1: 2), and a mol ratio of perfluoroalkyl halide to the solvent is (1: 5) to (1: 15); and after a reaction product is obtained upon completion of the reaction, cooling the reaction product to room temperature and distilling the reaction product to obtain perfluoroalkane. The method provided by the invention has the advantages of simple equipment, high operation security, etc.
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Paragraph 0028; 0029
(2016/11/28)
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- Synthesis of 2-(perfluoroalkyl)ethyl potassium sulfates based on perfluorinated Grignard reagents
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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.
- Paterová, Jana,Skalicky, Martin,Rybá?ková, Markéta,Kví?alová, Magdalena,Cva?ka, Josef,Kví?ala, Jaroslav
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experimental part
p. 1338 - 1343
(2011/02/22)
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- Bis(perfluoroorganyl)bromonium salts [(RF)2Br]Y (RF = aryl, alkenyl, and alkynyl)
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Bromonium salts [(RF)2Br]Y with perfluorinated groups RFC6F5, CF3CFCF, C 2F5CFCF, and CF3C≡C were isolated from reactions of BrF3 with RFBF2 in weakly coordinating solvents (wcs) like CF3CH2CHF2 (PFP) or CF3CH2CF2CH3 (PFB) in 30-90% yields. C6F5BF2 formed independent of the stoichiometry only [(C6F5)2Br][BF 4]. 1:2 reactions of BrF3 and silanes C6F 5SiY3 (Y = F, Me) ended with different products - C 6F5BrF2 or [(C6F5) 2Br][SiF5] - as pure individuals, depending on Y and on the reaction temperature (Y = F). With C6F5SiF3 at ≥-30 °C [(C6F5)2Br][SiF5] resulted in 92% yield whereas the reaction with less Lewis acidic C 6F5SiMe3 only led to C6F 5BrF2 (58%). The interaction of K[C6F 5BF3] with BrF3 or [BrF2][SbF 6] in anhydrous HF gave [(C6F5) 2Br][SbF6]. Attempts to obtain a bis(perfluoroalkyl) bromonium salt by reactions of C6F13BF2 with BrF3 or of K[C6F13BF3] with [BrF2][SbF6] failed. The 3:2 reactions of BrF3 with (C6F5)3B in CH2Cl2 gave [(C6F5)2Br][(C6F 5)nBF4-n] salts (n = 0-3). The mixture of anions could be converted to pure [BF4]- salts by treatment with BF3·base.
- Frohn, Hermann-Josef,Giesen, Matthias,Welting, Dirk,Bardin, Vadim V.
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experimental part
p. 922 - 932
(2010/10/03)
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- An improved procedure for the synthesis of perfluoroalkylacetylenes
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A new and easy way to synthesize acetylene compounds is proposed. This synthesis is improved by including in one-pot, three reactions in a single step, with good yields. The reactants are commonly used compounds.
- Calleja-Rubio,Crette,Blancou
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p. 361 - 364
(2007/10/03)
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- A Lewis acid catalytic process for preparing fluorocarboxylic acid halides
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Selected Group III and Group V Lewis acids were found to catalyze the isomerization and rearrangement of halosulfonyldifluoromethyl group (Rf-CF2SO2X, where X is either chlorine or fluorine) to form fluorocarboxylic acid halides (RfCOX). Fluorodesulfoxylation of the halosulfonyldifluoromethyl group yielded SOF2 as one of the two sulfur-containing oxides. Product analysis would suggest that both Lewis acid catalyzed and halogen exchange reactions are occurring and are dependent upon the starting halosulfonyldifluoromethyl material and Lewis acid.
- Behr,Cheburkov
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p. 369 - 372
(2007/10/03)
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A new synthesis of perfluoroalkylmethyloxiranes and perfluoroalkylmethylaziridines is accomplished by addition of allylalcohol or allylamine to iodoperfluoroalkanes in the presence of potassium or sodium hydroxide.
- Rubio,Blancou,Commeyras
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- Fluorinated poly(ether sulfones)
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Polymers comprising fluorine-containing poly(ether sulfones) and monomers comprising aromatic fluorine-containing sulfones used in the preparation of these polymers.
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- Kinetics and Mechanism of the Thermal Reaction between Perfluorobutene-2 and Trifluoromethylhypofluorite
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The kinetics of the thermal reaction between CF3OF and C4F8 have been investigated in the range of 30 deg C to 90 deg C.It was found to be a homogeneous chain reaction of moderate length.The main product is CF3CF(OCF3)CF2CF3, accompanied by small amounts of C8F18, CF3OOCF3 and CF3CF(OCF3)CF(OCF3)CF3 in constant ratio.Traces of (CF3CF(OCF3)CFCF3)2 are also formed.Inert gases and reaction products have no influence on the reaction, whereas small amounts of oxygen change its course.Under conditions in which / > 1, the reaction follows a second order rate expressi on - = k.The following mechanism explains the experimental results .The chain length ν = /2 is found to be ν = 19+/-3 in the range 32 deg C to 92 deg C, the rate constant of the starting reaction k1 = (5.34+/-0.30)106exp(-13.9 kcal*mol-1/RT)l*mol-1*s-1. - Keywords: Kinetics / Thermal reaction / Perfluorobutene-2 / Trifluoromethylhypofluorite / Perfluoroalkyl radicals
- Santos Afonso, M. dos,Schumacher, H. J.
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- FREE RADICAL CHEMISTRY, PART 5. A NEW APPROACH TO THE SYNTHESIS OF PERFLUORINATED ETHERS
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Fluorinations of the free-radical adducts of fluorinated alkenes, to ethers, over cobalt trifluoride are described and perfluorinated ethers are obtained at temperatures in excess of 400 deg C.The effect of structure on the formation of perfluoroethers is outlined.
- Chambers, Richard D.,Grievson, Brian,Drakesmith, Frederick G.,Powell, Richard L.
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p. 323 - 340
(2007/10/02)
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- THERMAL DECOMPOSITION OF PERFLUOROALKANESULFONYL FLUORIDES: THE PYROLYSIS OF PERFLUORO-n-OCTANE-1-SULFONYL FLUORIDE
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The preliminary data obtained from thermal decompositions of perfluoro-n-octane-1-sulfonyl fluoride in a continuous tubular-flow reactor are reported.The pyrolysis results in a radical reaction producing fluorocarbons, with high conversions and with yields depending on the experimental conditions.The reaction mixture composition also depends on the experimental conditions, so it is possible to obtain a prevalent formation of either light or heavy fluorocarbons.
- Napoli, M.,Fraccaro, C.,Scipioni, A.,Armelli, R.
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p. 377 - 386
(2007/10/02)
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- REACTIVITE DES PERFLUOROIODOALCANES AVEC LES CARBONATES ET PYROCARBONATES D'ALCOYLES EN PRESENCE DE COUPLE METALLIQUE ZINC-CUIVRE
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Perpluoroalkyl iodides RFI, in dissociating solvents, in the presence of zinc-copper couple give perfluoroorganic compounds RFZnI, which reac with alkyl carbonates and pyrocarbonates to give perfluorocarboxylic acids and perfluorocarboxylis esters of industrial interest.
- Benefice, S.,Blancou, H.,Commeyras, A.
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p. 1541 - 1544
(2007/10/02)
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