700-16-3Relevant articles and documents
Burdon, J.,Gilman, D. J.,Patrick, C. R.,Stacey, M.,Tatlow, J. C.
, p. 231 - 232 (1960)
Method for preparing 2, 3, 5-trichloropyridine on basis of layered manganese oxide catalysts with nanometer zinc
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Paragraph 0025; 0029; 0033; 0037; 0039; 0041; 0045; 0048, (2018/05/16)
The invention provides a method for preparing 2, 3, 5-trichloropyridine on the basis of layered manganese oxide catalysts with nanometer zinc. The method includes steps of dissolving manganese nitrateand zinc acetate in water, uniformly mixing the manganese nitrate and the zinc acetate with each other to obtain first liquid, dropwise adding alkali liquor into the first liquid to obtain second liquid, stirring and precipitating the second liquid to obtain manganese/iron mixed precipitates, adding the manganese/iron mixed precipitates into potassium permanganate solution to obtain third liquid,oxidizing the third liquid, filtering and washing the third liquid, adding carbon powder into the third liquid to obtain mixtures and calcining the mixtures at the high temperatures to obtain the layered manganese oxide catalysts with the nanometer zinc; carrying out reaction on pentafluoropyridine, DMF (dimethyl formamide) and active potassium fluoride powder under the effects of the layered manganese oxide catalysts with the nanometer zinc under strong-alkali conditions, filtering reaction products, and adding filter cake into calcium fluoride solution to obtain the 2, 3, 5-trichloropyridine on the basis of the layered manganese oxide catalysts with the nanometer zinc. The pentafluoropyridine is used as a raw material, the DMF is used as a solvent, and the active potassium fluoride powder is used as fluorinating agent. The method for preparing the 2, 3, 5-trichloropyridine on the basis of the layered manganese oxide catalysts with the nanometer zinc has the advantages that the reaction is mild and is high in efficiency, and the 2, 3, 5-trichloropyridine which is a product prepared by the aid of the method is high in purity.
From hypervalent xenon difluoride and aryliodine(III) difluorides to onium salts: Scope and limitation of acidic fluoroorganic reagents in the synthesis of fluoroorgano xenon(II) and iodine(III) onium salts
Abo-Amer, Anwar,Frohn, Hermann-Josef,Steinberg, Christoph,Westphal, Ulrich
, p. 1311 - 1323 (2008/12/21)
Fluorinated organodifluoroboranes RfBF2 are in general suitable reagents to transform XeF2 and RIF2 into the corresponding onium tetrafluoroborate salts [RfXe][BF4] and [R(Rf)I][BF4], respectively. (4-C5F4N)BF2 and trans-CF3CF{double bond, long}CFBF2 which represent boranes of high acidity form no Xe-C onium salts in reactions with XeF2 but give the desired iodonium salts with RIF2 (R = C6F5, o-, m-, p-C6FH4). The reaction of (4-C5F4N)BF2 with XeF2 ends with a XeF2-borane adduct. C6F5Xe(4-C5F4N), the first Xe-(4-C5F4N) compound, was obtained when C6F5XeF was reacted with Cd(4-C5F4N)2. We describe the synthesis of (4-C5F4N)IF2 and reactions of (4-C5F4N)IF2 and C6F5IF2 with (4-C5F4N)BF2. Analogous to [(4-C5F4N)2I][BF4] and [C6F5(4-C5F4N)I][BF4] aryl(perfluoroalkenyl)iodonium salts [R(R′)I][BF4] were obtained from RIF2 (R = C6F5, o-, m-, p-C6FH4) and R′BF2 (R′ = trans-CF3CF{double bond, long}CF, CF2{double bond, long}CF). The gas phase fluoride affinities pF- of selected fluoroorganodifluoroboranes RfBF2 and their hydrocarbon analogs are calculated (B3LYP/6-31+G*) and discussed with respect to their potential to introduce Rf-groups into hypervalent EF2 bonds. Four aspects which influence the transformation of hypervalent EF2 bonds (E = Xe, R′I) under the action of Lewis acidic reagents RAFn-1 (A = B, P; n = 3, 5) into the corresponding [RE][AFn+1] salts are presented and the important role of the acidity is emphasized. Fluoride affinities may help to plan the introduction of organo groups into EF2 moieties and to expand the types of acidic reagents. Thus C6H5PF4 with a pF- value comparable to that of RfBF2 compounds is able to introduce the C6H5 group into RIF2 (R = C6F5, p-C6FH4).