- 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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- Method for synthesizing perfluorobutyl methyl ether
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The invention relates to a method for synthesizing perfluorobutyl methyl ether, belonging to the field of organic chemical synthesis. The method for synthesizing perfluorobutyl methyl ether in the invention is characterized by comprising the following steps of: 1, subjecting carbon tetrachloride (with a molecular formula of CCl4) and pentachloropropylene (with molecular formula of CCl3CH=CCl2) toreacting under the action of a telomerization catalyst to generate nonachlorobutane (with a molecular formula of CCl3CH(CCl3)CCl3); 2, carrying out gas-phase catalytic dehydrochlorination on the nonachlorobutane under the action of a catalyst to generate perchlorobutene (CCl3C=(CCl2)Cl3); 3, subjecting the perchlorobutene and anhydrous hydrogen fluoride (AHF) to reacting under the action of a catalyst to generate hexafluorodichlorobutene (CF3C=(CCl2)CF3); 4, carrying out telomerization on hexafluorodichlorobutene, methanol (CH3OH) and potassium hydroxide to generate hexafluoromonochloroisopropenyl methyl ether (CH3O(C1)C=C(CF3)2); and 5, carrying out gas phase catalysis on hexafluoromonochloroisopropenyl methyl ether, chlorine and anhydrous hydrogen fluoride under the action of a catalystto synthesize perfluorobutyl methyl ether (CH3O(F2)C-C(CF3)2). According to the invention, raw materials are cheap and convenient to obtain; the catalysts have good stability and long service life; product separation and purification are simple; and industrial production can be easily implemented.
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Paragraph 0025; 0039-0041; 0055-0056
(2020/12/10)
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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 0088-0089
(2019/07/29)
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- Process for preparing hydrofluoroethers
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Process for obtaining hydrofluoroethers of formula (I):A-(Rf)n0-CF(Rf1)-O-Rh wherein:n0 is zero or 1; Rf is a bivalent radical: C1-C20 (per)fluoroalkylene, optionally containing one or more oxygen atoms;-CFW'O-(Rf2)-CFW-, wherein W and W', equal or different, are F, CF3; Rf2 is a (per)fluoropolyoxyalkylene;Rf1 is F or a C1-C10 (per)fluoroalkyl or (per)fluorooxyalkyl radical;Rh is a C1-C20 linear, branched, saturated or unsaturated alkyl, or C7-C20 alkylaryl,A = F, (Rh2O)-CF(Rf4)-, -C(O)F, wherein Rh2, equal to or different from Rh, has the Rh meanings and Rf4, equal to or different from Rf1, has the Rf1 meanings; wherein a mono- or bifunctional carbonyl compound of formula (IV) :B-Rf-C(O)Rf1B being F or -C(O)Rf4, Rf, Rf1 and Rf4 being as above, is reacted with at least one equivalent of a fluoroformate of formula (III) :R-OC(O)F ???wherein R = Rh or Rh2 as above defined; in the presence of an ion fluoride compound (catalyst) and of a dipolar aprotic organic compound, liquid and inert under the reaction conditions.
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- Process for preparing hydrofluoroethers
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Process for obtaining hydrofluoroethers of formula (I): A-(Rf)n0—CF(Rf1)—O—Rh??(I) wherein: n0 is zero or 1; Rf is a bivalent radical: C1-C20 (per)fluoroalkylene, optionally containing one or more oxygen atoms; —CFW′O—(Rf2)—CFW—, wherein W and W′, equal or different, are F, CF3; Rf2 is a (per)fluoropolyoxyalkylene; Rf1 is F or a C1-C10 (per)fluoroalkyl or (per)fluorooxyalkyl radical; Rh is a C1-C20 linear, branched, saturated or unsaturated alkyl, or C7-C20 alkylaryl, A═F, (Rh2O)—CF(Rf4)—, —C(O)F, wherein Rh2, equal to or different from Rh, has the Rh meanings and Rf4, equal to or different from Rf1, has the Rf1 meanings; wherein a mono- or bifunctional carbonyl compound of formula (IV): B—Rf—C(O)Rf1??(IV) B being F or —C(O)Rf4, Rf, Rf1 and Rf4 being as above, is reacted with at least one equivalent of a fluoroformate of formula (III) R—OC(O)F??(III) wherein R═Rh or Rh2 as above defined; in the presence of an ion fluoride compound (catalyst) and of a dipolar aprotic organic compound, liquid and inert under the reaction conditions.
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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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