76-04-0Relevant articles and documents
Synthesis production process of difluorochloroacetic acid
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Paragraph 0015-0021, (2017/05/10)
The invention discloses a synthesis production process of difluorochloroacetic acid, comprising the following steps: charging sulfur trioxide with nitrogen gas into an oxidation reaction kettle by an intermittent process, starting stirring; after reaching a certain temperature, adding difluorotetrachloroethane and catalyst according to a predetermined ratio into the oxidation reaction kettle; heating for reaction, observing the backflow condition, starting steaming the byproduct sulfuric chloride when the kettle temperature rises to a certain temperature while the backflow is small; after steaming the byproduct sulfuric chloride, carrying out charging for the second time; carrying out three-stage spray hydrolysis and absorption on the product difluorochloracetyl chloride to generate crude product difluorochloroacetic acid, and carrying out defluorination and rectification on the crude product to obtain finished product difluorochloroacetic acid. The synthesis production process of difluorochloroacetic acid disclosed by the invention adopts the difluorotetrachloroethane as a raw material, the finished product difluorochloroacetic acid is prepared by oxidation reaction, the preparation process has reasonable design, high absorption rate, high overall yield and low energy consumption; and the byproduct can be hydrolyzed and reused, so that the production process is clean, environment-friendly, safe and reliable.
Atmospheric sink of methyl chlorodifluoroacetate and ethyl chlorodifluoroacetate: Temperature dependent rate coefficients, product distribution of their reactions with Cl atoms and CF2ClC(O)OH formation
Blanco, María B.,Barnes, Ian,Wiesen, Peter,Teruel, Mariano A.
, p. 51834 - 51844 (2016/06/14)
Rate coefficients as a function of temperature have been measured for the first time for the gas-phase reactions of chlorine atoms with methyl chlorodifluoracetate (k1) and ethyl chlorodifluoroacetate (k2) using the relative rate technique. The experiments were carried out in a 1080 L photoreactor over the temperature range 287-313 K at a total pressure of 1000 ± 10 mbar of synthetic air using in situ FTIR spectroscopy to monitor reactants and products. The following Arrhenius expressions were obtained: k(MCDFA+Cl) = (9.6 ± 5.1) × 10-12exp[-(1363 ± 79)/T] and k(ECDFA+Cl) = (64.4 ± 29.7) × 10-12exp[-(1110 ± 68)/T]. The kinetic results are compared with previous experimental and theoretical studies. In addition, a product study of the reactions of Cl with methyl chlorodifluoracetate and ethyl chlorodifluoroacetate is reported. The results indicate that in the absence of NOx the main fate of the alkoxy radicals formed after H-atom abstraction by Cl from the -CH3 group in methyl chlorodifluoroacetate is reaction of the radical with O2 to form the mixed anhydride CF2ClC(O)OC(O)H. In the case of ethyl chlorodifluoroacetate the main fate of the alkoxy formed via H-atom abstraction by Cl from the -CH2- entity in the ethyl group is α-ester rearrangement to produce chlorodifluoroacetic acid and the corresponding radical. The yields of chlorofluoracetic acid (CF2ClC(O)OH) obtained were as follows: (34 ± 5)% and (86 ± 8)% for the reactions of Cl with CF2ClC(O)OCH3 and CF2ClC(O)OCH2CH3, respectively. The measured yields are rationalized in terms of mechanisms consisting of competitive reaction channels for the formed products in the oxidation, i.e. reaction with O2, α-ester rearrangement and a decomposition pathway. Atmospheric implications are discussed according to the rate coefficients obtained as a function of temperature and altitude, and regarding the formation of chlorofluorocarboxylic acid.
Preparation and properties of two novel selenoacetic acids: HCF 2C(O)SeH and ClCF2C(O)SeH
Gomez Castano, Jovanny A.,Romano, Rosana M.,Beckers, Helmut,Willner, Helge,Della Vedova, Carlos O.
body text, p. 2608 - 2615 (2012/05/04)
The novel selenocarboxylic Se-acids, HCF2C(O)SeH and ClCF 2C(O)SeH, were prepared by treating the corresponding carboxylic acids with Woollins' reagent. The boiling points were extrapolated from the vapor pressure curves to be 364 and 359 K for HCF2C(O)SeH and ClCF2C(O)SeH, respectively. Both compounds are unstable at ambient temperatures and decompose to the corresponding seleno anhydrides and release of H2Se. Hydrolysis results in formation of the carboxylic acids and hydrogen selenide, while diselenides presumably are obtained by oxidation. The conformational properties of these acids were studied by vibrational spectroscopy in combination with ab initio and DFT methods. IR vapor-phase spectra, Raman spectra of the neat liquids, and IR spectra of the Ar-matrix-isolated compounds deposited at two different nozzle temperatures were interpreted in terms of quenching conformational equilibria. The most stable structure of both acids was found to be syn-gauche in equilibrium with a second anti-syn form in HCF2C(O)SeH and with another two conformers, anti-gauche and anti-syn, in ClCF2C(O)SeH.
PENTACYCLIC ANION SALT AND USE THEREOF AS AN ELECTROLYTE
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, (2012/01/12)
The invention relates to a pentacyclic anion salt and to the use thereof in electrolyte compositions. The compound comprises an inorganic, organic or organometallic cation M of valency m (1≦m≦3) and m anions corresponding to the formula (I) in which Rf is a —CFZ′Z″ group in which Z′ is F or a perfluoroalkyl group having from 1 to 3 carbon atoms, and Z″ is an H, F or Cl group, an optionally fluorinated or perfluorinated alkoxy group having from 1 to 5 carbon atoms, an optionally fluorinated or perfluorinated oxaalkoxy group having from 1 to 5 carbon atoms or an optionally fluorinated or perfluorinated alkyl group having from 1 to 5 carbon atoms; Z″ being other than F when Z′ is F. An electrolyte composition comprises said salt in solution in a liquid solvent or a polymer solvent.
Preparation of compounds comprising a CHF2 or CHF group
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Page/Page column 2; 3, (2008/06/13)
Producing compounds (I) with a mono- or difluoromethyl group from compounds (II) with a mono- or difluorohalomethyl group, where halo is bromo, iodo or preferably chloro, comprises reacting (II) with zinc in the presence of an alcohol. An independent claim is also included for an azeotropic mixture of methyl difluoroacetate and methanol.
Methods for treating retroviral infections
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, (2008/06/13)
The present invention provides compounds for treating or preventing an HIV infection, or treating AIDS or ARC comprising administering a compound according to formula I where Ar, R1-R5, R11c and X1 are as defined herein.
Reductive alkylation of perfluorocarboxylic acid esters with CCl 3F or CCl4 and synthesis of higher linear perfluoroketones
Zeifman, Yu.V.,Postovoi
, p. 1815 - 1819 (2007/10/03)
Barbier-type reductive alkylation of perfluorocarboxylic acid esters (I) with CFCl3 and activated Al was successfully performed to give α,α-dichloroperfluoroketones (II). A similar reaction of CF 3COOEt with CCl4 and Al provided a convenient synthesis of CF3COCCl3. Ketones (II) were fluorinated further with SbF5 to form higher linear perfluoroketones (IX). An alternative approach to the synthesis of ketones (IX) was proposed by reductive perfluoroalkylation of esters (I) under the action of RFI and Al.
Reaction of Perfluoroalkanesulfinates with Allyl and Propargyl Halides. A Convenient Synthesis of 3-(Perfluoroalkyl)prop-1-enes and 3-(Perfluoroalkyl)allenes
Hu, Chang-Ming,Qing, Feng-Ling,Huang, Wei-Yuan
, p. 2801 - 2804 (2007/10/02)
The reaction of perfluoroalkanesulfinates, RfCF2SO2Na, with allyl and propargyl halides, in the presence of (NH4)2S2O8, gave 3-(perfluoroalkyl)prop-1-enes (RfCH2CH=CH2) and 3-(perfluoroalkyl)allenes (RfCH=C=CH2), respectively, in good yield.Evidence is presented for a radical addition-elimination mechanism for the reaction.The reaction represents a synthetically viable and convenient route to such compounds.
REACTIONS OF PERHALOCARBONS. PART IX. CONVERSION OF PER(POLY)FLUOROALKYL HALIDES INTO THE CORRESPONDING CARBOCYCLIC ACIDS WITH A REDOX SYSTEM
Hu, Chang-Ming,Qing, Feng-Ling,Zhang, Hong-Gen
, p. 275 - 280 (2007/10/02)
The conversion of per(poly)fluoroalkylhalides into the corresponding carbocyclic acids with a redox system-(NH4)2S2O8/HCO2Na is described.The reaction provides a convenient method for the synthesis of various per(poly)fluorocarboxylic acids under mild conditions.
Process for the preparation of fluorocarboxylic acids
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, (2008/06/13)
Fluorocarboxylic acids are prepared by metering fluoronitroaliphatic compounds into a mineral acid which has been initially introduced.
