46 results about "Tetrakis(triphenylphosphine)palladium(0)" patented technology

The invention relates to a preparation method of a phosphinobenzene compound. The method is characterized in that a bromobenzene compound reacts with magnesium to prepare a Grignard reagent, and the Grignard reagent reacts with a chlorophosphine compound under the catalysis of tetrakis(triphenylphosphine)palladium to obtain the phosphinobenzene compound. The method concretely comprises the following steps: preparing the Grignard reagent from the bromobenzene compound, magnesium chips and an organic solvent under the protection of insert gas, and refluxing for 2-10h; adding tetrakis(triphenylphosphine)palladium at room temperature, stirring for 10min-3h, adding the chlorophosphine compound at room temperature in a dropwise manner, and carrying out a refluxing reaction for 1-10h; and adding an aqueous solution of saturated weakly-acidic and weakly-alkaline salt to the above obtained reaction solution in a dropwise manner in ice-water bath, carrying out liquid separation, removing the solvent from the obtained organic phase, adding an alcohol solvent for crystallizing, and filtering obtained crystals to obtain the phosphinobenzene compound. The preparation method has the advantages of great increase of the preparation yield, simple post-treatment, omitting of the repeated ammonia water washing process, preparation process simplification, and facilitation of large-scale industrial production.

The invention discloses a method for synthesizing 1-chloro-2-bromobenzo[9,10]phenanthrene, which comprises the following steps: putting chlorobenzene and butanedioic anhydride into a reaction bulb, sufficiently stirring, adding HB(OH)2, heating to 40-50 DEG C, stirring uniformly, and standing to room temperature; adding 7.26g of 2-bromobenzaldehyde and 45mL of ethanol into the reaction bulb twice, stirring uniformly, adding 86.0g of 20% sodium carbonate water solution, quickly adding tetra(triphenylphosphine) palladium, heating from room temperature to 70-80 DEG C (under reflux), keeping stirring at such temperature to react for 6 hours, sampling, and carrying out HPLC (high performance liquid chromatography) central control; after the 2-bromobenzaldehyde is reacted completely, cooling the reaction solution to 25-30 DEG C, and dropwisely adding methanesulfonic acid at room temperature; and after the reaction finishes, adding potassium carbonate into the reaction bulb, carrying out phase splitting, filtering and precipitating the solid powder, wherein the yield is 60.12%, and the HPLC is 99.12%. The method avoids the problems of complex synthesis, incapability of mass production, environmental pollution, side reactions and the like in the traditional method.

The invention discloses a preparation method for an alkenyl phosphate compound. By taking palladium acetate or tetra(triphenylphosphine) palladium as a catalyst, an alkali, a ligand, a diazo compound and a halide or an alkali, tosylhydrazone and a halide react under protection of an N2 atmosphere in an organic solvent to obtain the alkenyl phosphate compound RR'C=C(Ar)(P(O)(OMe)2), wherein Ar represents substituted or unsubstituted aryl comprising phenyl, naphthyl and heterocyclic rings; R and R' represent substituted or unsubstituted aryl, alkyl, alkenyl or hydrogen. According to the reaction referred to the invention, an E-configuration alkenyl phosphate compound can be smoothly obtained. The preparation method is convenient and simple to operate and has good tolerance and universality on functional groups. Moreover, the use level of the catalyst is relatively small, neither the reagent nor the solvent is specially treated, and the reaction cost is relatively low, so that the preparation method can be widely used for preparing the alkenyl phosphate compound.

The present invention discloses a difluoropropargyl-containing compound, a preparation method and applications. The preparation method comprises that in the presence of an organic solvent, a catalyst, a ligand and an alkali, a compound A and a compound B are subjected to a coupling reaction to obtain a compound C, wherein the catalyst is one or a plurality of materials selected from palladium acetate, palladium trifluoroacetate, tetrakis(triphenylphosphine)palladium, tris(dibenzylideneacetone)dipalladium chloroform adduct, and tris(dibenzylideneacetone)dipalladium, and the ligand is one or a plurality of materials selected from triphenylphosphine, tris(o-methoxyphenyl)phosphine, tris(o-methylphenyl)phosphine, tri-tert-butylphosphine fluoroborate, 2-(dicyclohexylphosphino)-2'-methylbiphenyl, 2-(di-tert-butylphosphino)biphenyl, and 4,5-bisdiphenylphosphino-9,9-dimethyl xanthene. According to the present invention, the method has characteristics of low catalyst consumption, mild reaction condition, high region selectivity, wide application range, and high reaction yield, and is suitable for industrial production. The compounds A, B and C are defined in the specification.