- Preparation method of isolated hydrofluoroether
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The invention discloses a preparation method of isolated hydrofluoroether. The preparation method comprises the following steps: in the presence of inorganic fluoride and a co-catalyst, carrying out an alkylation reaction on perfluorinated epoxide and an alkylation reagent in an aprotic polar solvent to obtain the isolated hydrofluoroether. The main raw material perfluorinated epoxide can be prepared by epoxidation of perfluoro-olefin, the raw materials are simple and easy to obtain, the cost is lower than that of perfluorohexanone and perfluoroacyl fluoride compounds, the stability is good, the subsequent reaction is facilitated, and the quality can be ensured. The preparation method has the advantages that the reaction speed is high, the reaction time is short, the raw materials can be completely converted within 3-5 hours, the residual quantity of the raw material perfluorinated epoxy compound in the obtained crude product can be as low as 0.1% or below, and the reaction conversionrate is high. The content of the target product can reach 97% or above, the reaction selectivity is high, the byproducts are few, and the method is suitable for industrial application.
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Paragraph 0021; 0022; 0069; 0070
(2021/03/05)
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- Method for preparing fluorine-containing ether
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The invention relates to a 'method for preparing fluorine-containing ether', and belongs to the field of chemical synthesis. The method comprises the steps that under a nitrile solvent condition, carbonyl fluoride, trifluoroacetyl fluoride, pentafluoropropionyl fluoride, heptafluoro-n-butyryl fluoride, heptafluoro-iso-butyryl fluoride and other acyl fluorides are taken as raw materials to have anaddition reaction with metal fluorides to obtain perfluoroalkoxide, then under water catalysis, the perfluoroalkoxide and a low-toxic or even non-toxic harmless alkylating agent are subjected to an alkylation reaction to obtain the fluorine-containing ether. The method for preparing the fluorine-containing ether has the advantages that not only is the reaction condition mild, the yield of the fluorine-containing ether is high, but also the low-toxic or even non-toxic harmless alkylating agent is taken as a safe alkylation agent, the process is safe and reliable, and effective separation can beperformed by an ordinary distillation means in the industry.
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Paragraph 0084-0085
(2019/07/29)
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- Hydrofluoroether synthetic method
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The invention discloses a hydrofluoroether synthetic method which comprises the following steps of throwing vinyl ether, a solvent and a composite fluoride agent in a reactor, rising the temperature to a temperature required for reaction to perform reaction, and separating a reaction liquid to obtain a hydrofluoroether product, wherein the molar ratio of the vinyl ether, the solvent and the composite fluoride agent is 1 to (1-3) to (1-2), the reaction temperature is 50-150 DEG C, and the reaction time is 2-5h. According to the hydrofluoroether synthetic method provided by the invention, the composite fluoride agent is used to perform synthesis of the hydrofluoroether, fluorination addition can be efficiently performed at lower temperature, the yield is larger than 90 percent, and the deficiencies of the traditional synthetic technology are effectively solved.
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Paragraph 0037; 0038
(2018/06/26)
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- New catalytic alkylation of in situ generated perfluoro-alkyloxy-anions and perfluoro-carbanions
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Alkyl fluoroformates RHOC(O)F are a new family of excellent alkylating agents. Perfluoroacyl fluorides, selected perfluoroketones and fluoroolefins can be alkylated to hydrofluoroethers RF-O-R H and hydrofluoroalkanes RF-RH, respectively. Potassium fluoride and cesium fluorides catalysts in glymes at 50-100°C are the preferred experimental conditions.
- Galimberti, Marco,Fontana, Giovanni,Resnati, Giuseppe,Navarrini, Walter
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p. 1578 - 1586
(2007/10/03)
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- Methyl hypofluorite (MeOF) reactions with various fluoroolefins
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The reaction of methyl hypofluorite (MeOF) with certain fluoroolefins, such as CF2=CF2, CF2=CFCF3, CF2=CFOCF3, CF2=CFOMe, CF2=CClF, CF2=CHF, CF2=CH2, CHF=CH2, CF2=CFCF=CF2, occurred in CD3CN or in the presence of NaF. Using neat MeOF in the presence of NaF was a novel method and gave good results. We observed that when more than three fluorine atoms are bonded to the C-C double bond, the addition products were obtained in mostly good yields.
- Suzuta, Tetsuya,Abe, Takashi,Sekiya, Akira
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- Perfluoroalcohols
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Perfluorinated primary alcohol adducts with triethylamine were prepared from lower perfluorinated acid fluorides and triethylamine monohydrofluoride. They are stable compounds and may be used as a source of RFO groups in organic syntheses.
- Cheburkov, Yuri,Lillquist, Gerald J.
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p. 123 - 126
(2007/10/03)
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- New synthetic method of alkyl perfluoroalkyl ethers
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vic-Difluorination of alkyl perfluoroenol ethers proceeded with high- valence metal fluoride, such as cobalt (III) fluoride and potassium tetrafluorocobaltate, in good yields to afford alkyl perfluoroalkyl ethers.
- Tamura, Masanori,Takubo, Seij,Quan, Heng-Dao,Sekiya, Akira
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p. 343 - 344
(2007/10/03)
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- FLUOROALIPHATIC ESTERS OF FLUOROSULFONIC ACID. 2. REACTION BIS(FLUOROSULFATO)PERFLUOROALKANES WITH CESIUM FLUORIDE
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2,3-Bis(fluorosulfato)perfluoroalkanes split under the action of CsF in the absence of solvents, giving a mixture of α-fluorosulfatoperfluoro ketones, perfluoroalkene sulfates, and perfluoro α-diketones.The occurence of these reactions in solutions results mainly in the formation of oxides of the corresponding fluoroolefins or products of their conversions.The reactions carried out are the first examples of nucleophilic substitution at a secondary carbon atom in a perfluorinated saturated chain.
- Rogovik, V. M.,Delyagina, N. I.,Mysov, E. I.,Cherstkov, V. F.,Sterlin, S. R.,German, L. S.
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p. 1870 - 1876
(2007/10/02)
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