- Continuous preparation method of hexafluoropropylene trimer
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The continuous preparation method comprises the following steps: in a microchannel reactor, a liquid phase catalyst preheated by hexafluoropropylene and a preheating module is reacted at 70 - 140 °C to obtain a hexafluoropropylene trimer. The liquid phase catalyst is prepared from component A, component B, component C and component D. The component A is at least one selected from the group consisting of potassium fluoride, cesium fluoride, and potassium hydrofluoride. The component B is selected from at least one 18 - crown ether -6, β - cyclodextrin and polyethylene glycol. The component C is selected from at least one of a nitrile compound, a glycol ether compound and an amide compound. The component D is selected from at least one of-4 -methyl -2 - pentene,2 - methyl -2 - pentene,2 - ethyl -3 and 3 -dimethylethylene oxide. The continuous preparation method has the advantages of accurate temperature control, good selectivity, continuous feeding, reusability of the catalyst and the like.
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Paragraph 0048-0051; 0055
(2021/10/27)
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- Continuous preparation method of high-purity perfluoro-2, 4-dimethyl-3-heptene
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The invention discloses a continuous preparation method of high-purity perfluoro-2, 4-dimethyl-3-heptene. The preparation method comprises the following step: in a micro-channel reactor, hexafluoropropylene and a liquid phase catalyst preheated by a preheating module react at 70-140 DEG C to obtain the perfluoro-2, 4-dimethyl-3-heptene. the liquid-phase catalyst is prepared from a component A, a component B, a component C and a component D, the component A is selected from at least one of potassium fluoride, cesium fluoride and potassium bifluoride; the component B is selected from at least one of crown ether, cyclodextrin, polyethylene glycol, calixarene or pillararene; the component C is an amide compound; and the component D is selected from at least one of perfluoro-4-methyl-2-pentene, perfluoro-2-methyl-2-pentene and perfluoro-2-ethyl-3, 3-dimethyl ethylene oxide. The method has the advantages of accurate temperature control, good selectivity, high product purity and the like.
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Paragraph 0038-0053; 0062-0071
(2021/10/27)
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- Synthesis of highly branched perfluoroolefins that are super-congested via multi-substitution of trifluoromethyl groups: Trifluoromethylation of hexafluoropropene trimers with Ruppert-Prakash reagent
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The reaction of hexafluoropropene trimers with Ruppert-Prakash (CF3SiMe3) reagent gave highly congested perfluoroolefins such as the mono-trifluoromethylation products F-2,4-dimethyl-3-isopropyl-2-pentene (P1) and E- and Z-forms of F-4,4-dimethyl-3-isopropyl-2-pentene (2E and 2Z), and the bis-trifluoromethylation product F-2,4,4-trimethyl-3-isopropyl-2-pentene (3). The E-form of 2 was also comprised of two rotamers. Various aprotic polar solvents were surveyed for this reaction, and it was found that the aprotic solvent DMI has a unique solvent effect to selectively give the mono-trifluoromethylated perfluoroolefin P1, a precursor for the persistent perfluoroalkyl radical F-3-isopropyl-2,4-dimethyl-3-pentyl, in very high yield.
- Ono, Taizo
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p. 128 - 134
(2017/04/18)
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- Persistent perfluoroalkyl radical investigations under reductive environment: Reaction with electron-donating reagents
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The reactivity of persistent perfluoroalkyl radical, perfluoro-3-ethyl-2,4-dimethyl-3-pentyl (1), with various electron-donating reagents was investigated. It is revealed that 1 which is robust under oxidative conditions is rather vulnerable under reductive conditions. Thus, Lewis bases such as triethylamine and triphenylpnictogens (Ph3Pn, Pn=N, P, As, Sb, Bi) and some soft anions such as iodide or tetraphenyl borate reacted with 1 to give perfluoro-3-isopropyl-4-methylpent-2-ene (2) quantitatively. Even very weak Lewis bases such as diethyl ether and diethylsulfide also reacted with 1 to give 2 and additionally a hydrido product, perfluoro-3-ethyl-3-H-2,4-dimethylpentane (4). Hydrogen gas did not react with 1 at all without a catalyst, but in the presence of metal Pd adsorbed on charcoal, smoothly reacted to give 2 in quantitative yield. Metal hydrides such as LiAlH4, NaBH4, NaH, BH3 (THF complex), Bu3SnH, Me2PhSiH reacted with 1 to give 2 and 4. That an electron transfer mechanism is operating in the formation of 2 is obvious, but not conclusive in the formation of 4.
- Ono, Taizo,Fukaya, Haruhiko,Hayashi, Eiji,Saida, Hiroko,Abe, Takashi,Henderson, Philip B.,E. Fernandez, Richard,Scherer, Kirby V.
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p. 173 - 182
(2007/10/03)
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- Stable Perfluoroalkyl Carbanion Salts
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The synthesis and properties of tris(dimethylamino)sulfonium (TAS) salts of perfluoro tertiary carbanions are desribed.Many of these unique salts are isolable and stable up to their melting points, and they dissolve in organic solvents to provide high concentrations of perfluoro carbanions.Several reactions of TAS+CF3CF2CF2C-(CF3)2, which exemplify the synthetic utility of these new salts, are reported.
- Smart, Bruce E.,Middleton, William J.,Farnham, William B.
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p. 4905 - 4907
(2007/10/02)
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- OLIGOMERIZATION OF PERFLUOROPROPYLENE CATALYZED BY ?-BIS(ARENE)CHROMIUM(0) COMPLEXES
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Oligomerization of perfluoropropylene catalyzed by four ?-bis(arene)chromium(0) complexes (arene = benzene, diphenyl, 1,3,5-trimethylbenzene and hexamethylbenzene) were compared.Besides dimers (I, II) and trimers (III, IV) reported previously , two defluorotrimers VA and VB were found to be present in the oligomer mixtures.The formation of VA and VB was shown to be derived from trimer IV by hydrogenation followed by elimination of two moles of hydrogen fluoride.
- Huang, Yaozeng,Li, Jisen,Zhou, Jianqiang,Wang, Qiwen,Gui, Meimei
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p. 169 - 175
(2007/10/02)
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- ?-BIS(BENZENE)CHROMIUM(0)-CATALYZED OLIGOMERIZATION OF PERFLUOROPROPYLENE
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In the presence of zerovalent ?-bis(benzene)chromium(0) (I), perfluoropropylene (II) was found to undergo oligomerization under very mild conditions to dimers (b.p. 46 deg, M+, 300) and trimers (b.p. 100-102 deg C, M+ - 19, 431) in the ratio of 2.5-3.0 to 1.One mol of metal complex could catalyze the conversion of 50 mol of perfluoropropylene.One the basis of 19F NMR, the structures of the dimers are III and IV in a ratio of ca. 80/20 and the trimers V and VI; VII and VIII also seemed to be present.V/VI/(VII + VIII) is 80/10/4.In benzene solution, perfluoropropylene was shown not to be catalytically oligomerized by fluoride ion (KF, CrF2 of (CH3)4NF) (nor by monovalent ?-dibenzenechromium(I).A possible mechanism of the reaction was proposed.
- Huang, Yaozeng,Li, Jisen,Zhou, Jianqiang,Zhu, Zhongmu,Hou, Guoyu
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p. 185 - 191
(2007/10/02)
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