- Method for synthesizing beta-halogen tetrafluoroacyl fluoride
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The invention discloses a method for synthesizing beta-halogen tetrafluoroacyl fluoride. The preparation method specifically comprises the following steps: adding an alkali halide and a catalyst into a drying reactor with a dry ice reflux condenser, placing the drying reactor in an ice water bath, slowly introducing hexafluoropropylene oxide with stirring, keeping the drying reactor in the ice water bath for 2h until no reflux exists at the bottom of the dry ice reflux condenser, continuing performing stirring for 2h, separating liquid with a liquid separation funnel, performing distillation under normal pressure, introducing gas produced in a distillation process into a cold trap for collection, and transferring the gas into a steel bottle to obtain liquid beta-halogen tetrafluoroacyl fluoride. The conversion rate of the raw material and the purity of a product are high, the purity of the product subjected to fractional distillation can reach 99 percent or higher, the product can chemically react with alcohol to obtain ester with purity of 99 percent, the production steps of the preparation method are simple and safe, and the preparation method is short in reaction time and high in productivity.
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Sheet 0012; 0013; 0014
(2017/08/29)
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- Pyrolytic decarboxylation of some derivatives of perfluorinated mono- and dicarboxylic acids
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Pathways of pyrolysis of perfluorinated carboxylic acids are considered in relation to the structure of the acids and reaction conditions. The reaction mechanism is discussed.
- Lebedev,Berenblit,Starobin,Gubanov
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p. 1640 - 1645
(2007/10/03)
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- Reactions involving hexafluoropropylene oxide: Novel ring opening reactions and resolution of a racemic mixture of a bromofluoro ester, ultrasound mediated Reformatsky reactions and stereoselectivity
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A novel ring opening reaction of hexafluoropropylene oxide (HFPO) 1 with lithium bromide/zinc bromide and subsequent reaction of the resulting acyl fluoride with primary and secondary alcohols gave bromofluoro esters 2, 3, 4 and 7. Reaction of the corresponding acyl fluoride with water leads to acid 9 which on treatment with dehydroabietylamine 10 gave the diastereomeric salt 11. Resolution of 11 and subsequent hydrolysis and esterification reactions led to enantiomerically pure ester 12. Reformatsky reactions with 2 were studied which gave the alcohols 6 and 5. A Reformatsky reaction of 12 with formaldehyde afforded an alcohol 13 which is indicated by NMR spectroscopy in the presence of a chemical shift reagent to have proceeded stereoselectively.
- Coe, Paul L.,Loehr, Marianne,Rochin, Christophe
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p. 2803 - 2811
(2007/10/03)
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- Synthesis of functionalized polyfluoroalkyl hypochlorites and fluoroxy compounds and their reactions with some fluoroalkenes
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Several new polyfluoroalkyl hypochlorites and fluoroxy compounds containing Cl, H and Br in the alkyl group have been prepared and characterized by 19F NMR, 1H NMR and IR spectroscopies and by their reactions with fluoroalkenes to produce new polyfluoroethers.The novel compounds are prepared by the CsF-catalyzed addition of F2 or ClF to the C=O bond in CF3C(O)CF2Cl, ClCF2C(O)CF2Cl, and their derivatives HCF2C(O)CF3 and HCF2C(O)CF2Cl.Compounds containing an α-CF3 group exhibit enhanced thermal stability.New fluoroxy compounds and hypochlorites have also been prepared from the acid fluorides CF3-CFX-C(O)F (X = Cl, Br), which are obtained by the ring-opening reaction of hexafluoropropene oxide with (CH3)3SiCl, LiBr and (C2H5)3SiBr.These -OX compounds behave similarly to previously known materials with two α-F atoms, decomposing quickly at room temperature to COF2 and haloalkanes.
- Randolph, Bruce B.,DesMarteau, Darryl D.
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p. 129 - 150
(2007/10/02)
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- Halogen perchlorates. Additions to perhaloolefins
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The recently discovered halogen perchlorates, Cl2O4 and BrClO4, have been found to react with perhaloolefins by adding across the carbon-carbon double bond. These reactions proceeded quickly at low temperatures, in the absence of a solvent, to furnish the previously unknown perhaloalkyl perchlorates in high yield. Compounds prepared in this manner were ClCF2CF2ClO4, ClCF2CFClClO4, Cl2CFCFClClO4, CF3CFClCF2ClO4, BrCF2CFClClO4, and CF3CFBrCF2ClO4. Characteristic data for these surprisingly stable compounds are reported. All the new perchlorates reacted with alkali metal fluorides to form the corresponding acid fluorides and either FClO3 or mixtures of FClO3, Cl2, and O2.
- Schack, Carl J.,Pilipovich, Don,Hon, John F.
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p. 897 - 900
(2007/10/12)
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