60 results about "Tricyclohexylphosphine" patented technology

The invention discloses a complex and application of monophosphine monoazacyclo-carben nickel containing tricyclic hexyl phosphine. The molecular formula of the complex of the monophosphine monoazacyclo-carben nickel is (PCy3)Ni[(RNCHCHNR)C]X2; in the molecular formula, the PCy3 is tricyclic hexyl phosphine; the R is tertiary butyl, 2,6-diisopropyl phenyl or mesitylene; the X is chlorine or bromine. The complex of monophosphine monoazacyclo-carben nickel containing tricyclic hexyl phosphine is simple to prepare, easy to operate, easy in purification of products and high in yield, can stably exist in air, and can efficiently catalyze cross coupling reaction of aryl methyl ether and aryl Grignard reagent.

A polymerizable composition is obtained by mixing a metathesis polymerization catalyst including benzylidene(1,3-dimethyl-4-imidazolidin-2-ylidene)(tricyclohexylphosphine)ruthenium dichloride, a cycloolefin monomer such as 2-norbornene or tetracyclo[6.2.1.13,6.02,7]dodec-4-ene, a chain transfer agent such as allyl methacrylate, and hollow particles such as Shirasu balloons. A crosslinkable resin composite is obtained by coating or impregnating the polymerizable composition onto or into a support medium, and carrying out bulk polymerization of the polymerizable composition. A crosslinked resin composite is obtained by crosslinking the crosslinkable resin composite.

A method of controlled curing by a metathesis reaction upon mixing its components, the method including the step of mixing an olefin-containing substrate, a metathesis catalyst, and a reaction control agent. The metathesis catalyst is a ruthenium or osmium carbene complex catalyst, such as one containing an alkylidene ligand with basicity higher than that of tricyclohexylphosphine (PCy3) and a neutral electron donor ligand with a basicity lower than that of PCy3, whereby the catalyst initiates the metathesis reaction of the composition upon mixing with the substrate. The reaction control agent is effective to slow the progress of the metathesis reaction and prevent its completion in the absence of an elevated temperature. The control agent may be a hydrocarbon containing carbon-carbon double bonds and / or triple bonds, or maybe a modified hydrocarbon with one or more Group 14 or 15 atoms. Prior to catalyst deactivation, the mixture is exposed to an elevated temperature to accelerate the catalyst and allow the metathesis reaction to proceed toward completion.

The invention relates to a ruthenium carbene complex, a preparation method and an application thereof. The chemical formula of the ruthenium carbene complex is shown as formula (I), wherein X is selected from trifluoromethyl, nitryl, dimethylamino or cyanogroup. In a preparation process, firstly, chloromethyl benzene ligand reacts with zinc alkyls so as to synthesize a chloromethyl benzene-zinc alkyls compound, and then the chloromethyl benzene-zinc alkyls compound reacts with tris (triphenylphosphine) ruthenium chloride and tricyclohexylphosphine in turn so as to acquire a catalyst precursor, and lastly, the catalyst precursor and N-heterocyclic carbene are subjected to ligand replacement. The prepared ruthenium carbene complex is used as a catalyst for catalyzing the olefin metathesis. Compared with the prior art, the ruthenium carbene complex provided by the invention has the advantages of convenience in preparation, property stability and capability of effectively catalyzing the olefin metathesis. The preparation method is characterized by simple operation, technology stability, controllability, environment-friendly effect, high yield, suitability for industrial amplification production and wide application prospect.

The invention discloses a self-repairable photosensitive weld-retarding dry film. According to the invention, dicyclopentadiene and ethylidene norbornene are coated in microcapsule with the diameter of 1-10 [mu]m formed by urea-formaldehyde resin, the microcapsule is mixed with a carboxyl-containing alkali soluble polymer, a vinyl-containing unsaturated monomer or oligomer, a photoinitiator, an auxiliary agent, dicyclopentadiene, ethylidene norbornene, and bis(tricyclohexylphosphine)benzylidine ruthenium dichloride, a support is coated by a mixture and then dried; the upper layer is applied with a polymer cover membrane, and then the self-repairable photosensitive weld-retarding dry film is prepared. After a self-repairable material is introduced into the weld-retarding dry film, the weld-retarding dry film can realize self repairing when the defects of crack and cavity are generated, anti-welding performance and insulating property of a circuit board are guaranteed, and the usage life of the circuit board is greatly prolonged.

A polymerizable composition is obtained by mixing a metathesis polymerization catalyst including benzylidene(1,3-dimethyl-4-imidazolidin-2-ylidene)(tricyclohexylphosphine)ruthenium dichloride, a cycloolefin monomer such as 2-norbornene or tetracyclo[6.2.1.13,6.02,7]dodec-4-ene, a chain transfer agent such as allyl methacrylate, and hollow particles such as Shirasu balloons. A crosslinkable resin composite is obtained by coating or impregnating the polymerizable composition onto or into a support medium, and carrying out bulk polymerization of the polymerizable composition. A crosslinked resin composite is obtained by crosslinking the crosslinkable resin composite.

A composition curable by a metathesis reaction upon mixing its components and comprising an olefin-containing substrate, a metathesis catalyst, and a reaction control agent for slowing the progress of the metathesis reaction. The metathesis catalyst is a ruthenium or osmium curbene complex catalyst, such as one containing an alkylidene ligand with basicity higher than that of tricyclohexylphosphine (PCy3) and a neutral electron donor ligand with a basicity lower than that of PCy3, whereby the catalyst initiates the metathesis reaction of the composition upon mixing with the substrate. The reaction control agent is an organic compound that contains carbon-carbon double and / or triple bonds and one or more Group 14 atoms and is present in an amount effective to slow the progress of the metathesis reaction. The olefin containing substrate may be, for example, one or a combination of a di-, tri- or quadri-functional polydimethylsiloxane end-capped with norbornenylethyl groups or a polydimethylsiloxane tethered and end-capped with norbornenylethyl groups.

The invention belongs to the technical field of molecular probes, and discloses a probe with functions of successive imaging and killing of bacteria and cancer cells and application of the probe. Thestructure of the probe is shown as a formula I, wherein X is preferably hydrogen; Y is preferably a linking bond; Z is preferably O; R is preferably hydrogen; W is preferably absent; L is preferably aC1-C16 alkylene ether group; T<+> is one of tricyclohexylphosphine salt cations, triphenylphosphine salt cations and pyridine cations; and Q<-> is a monovalent anion. The probe disclosed by the invention is applied to preparation of antibacterial and / or anticancer drugs and preparation of a fluorescence imaging agent. The probe provided by the invention realizes dual effects of antibiosis and anticancer by increasing permeability of bacterial cell membranes and destroying the structure of mitochondria in cancer cells, and has successive imaging and killing functions of bacteria and cancer cells.

The invention relates to a norbornene, tetrafluoroethylene and N-phenyl maleimide ternary copolymerization catalyst and a ternary copolymerization method. The ternary copolymerization method is characterized by comprising the steps of dissolving bis(tricyclohexylphosphine)palladium dichloride and a ligand in a first solvent in a 3-mouth flask in a dry inert atmosphere so as to obtain a mixed solution; dripping titanium iso-propylate to the mixed solution at 150-250 rpm; after the dripping is finished, continuing to stir the materials at a temperature of 30-50 degrees centigrade for 30-50 minutes to obtain a palladium-titanium complex catalyst; taking and adding the norbornene, tetrafluoroethylene and N-phenyl maleimide monomers to a nitrogen charged high pressure kettle which is vacuumized for multiple times; adding a second solvent to the high pressure kettle to dissolve the monomers; and then adding the palladium-titanium complex catalyst to the high pressure kettle and enabling the materials in the high pressure kettle to react at a certain temperature and under a certain pressure; pouring a reaction product into ethanol solution containing hydrochloric acid; washing obtained precipitates by using ethanol to be neutral; and drying the washed precipitates in a vacuum manner to obtain a norbornene, tetrafluoroethylene and N-phenyl maleimide ternary copolymer.

The invention discloses a preparation method of a novel polysubstitution dihydropyrimidine indolone derivative, which belongs to the technical field of organic synthesis. The preparation method comprises the following steps: adding substitution N-methoxyindolamide into a reactor, substituting styrene, cobaltous acetate, silver acetate, sodium acetate, 4-methylpyridine and tricyclohexylphosphine, stirring in a solvent, after the reaction is finished, concentrating filtrate by using a rotary evaporator to obtain a crude product, separating the crude product by virtue of silica gel column chromatography to obtain a target compound. The synthetic method of the polysubstitution dihydropyrimidine indolone derivative provided by the invention has the characteristics of science, reasonability, simple synthetic method, high yield of target compounds, ease in purifying the product and the like. A reaction equation is shown in the description.

The invention discloses a 1,10-phenanthroline monohydrate-based main material, taking an aryl-substituted amino unit as the main material of a power supply unit. The invention also provides a preparation method of the main material, comprising the following steps: (1) preparing 9-(3-bromophenyl)carbazole; (2) preparing 9-(3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)carbazole; (3) under nitrogen protection, adding palladium acetate and tricyclohexylphosphine into a mixed solution of 3-bromo-1,10-phenanthroline, the 9-(3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)carbazole, a potassium carbonate aqueous solution, ethanol and toluene, and generating Phen-m-PhCz. The material is simple to synthetize and purify, has better solubleness and film form, is easy for hole and electron injection, and has important application prospect in organic electroluminescence devices.

The present invention belongs to the field of polymer materials, and particularly relates to a catalyst composition and a terpolymer synthesis method. The catalyst composition comprises a Schiff base trivalent cobalt compound, a Schiff base divalent cobalt compound and a co-catalyst, wherein the Schiff base trivalent cobalt compound is one or a plurality of materials selected from compounds represented by formulas I-III, the Schiff base divalent cobalt compound is one or a plurality of materials selected from compounds represented by formulas IV-VI, and the co-catalyst comprises one or a plurality of materials selected from bis(triphenylphosphine)iminium chloride, 4-dimethylamino pyridine, N-methylimidazole, tricyclohexylphosphine, tetramethylammonium bromide and tetrabutylammonium bromide. According to the present invention, by using the catalyst composition, propylene oxide, carbon dioxide and lactide can be synthesized into the copolymer having the gradual multi-block structure, wherein the glass transition temperature of the copolymer can be up to more than 50 DEG C. The formulas I-VI are defined in the specification.

The invention relates to a synthesis method of a ruthenium carbene catalyst, which comprises the following steps: (1) adding benzyl halide and triphenylphosphine into a reactor, reacting in a medium,and reacting the obtained reaction product under the action of a strong alkali to obtain a first intermediate product; (2) reacting the first intermediate product with triphenylphosphine ruthenium chloride in a solvent, replacing triphenylphosphine with tricyclohexylphosphine, filtering and washing to obtain a ruthenium carbene complex precursor; and (3) carrying out a complex addition reaction onthe ruthenium carbene complex precursor and a functional ligand to obtain the target product that is the ruthenium carbene catalyst. Compared with the prior art, the method has the characteristics ofcapability of efficiently controlling the reaction speed, short preparation period, simplicity in operation, stable process, environmental friendliness, good atom economy and the like, and has a relatively great application prospect in the aspect of industrial amplification.

The invention relates to a preparation method of a drug for treating chronic granulocytic leukemia, belonging to the field of medical chemistry, and specifically relates to a preparation method of 3-[2-(imidazo[1,2-b] pyridazine-3-yl) acetenyl]-4-methyl-N-{4-[4-methyl piperazine-1-yl] methyl}-3- trifluoromethyl phenyl} benzoyl amide (ponatinib). The method comprises the following steps: adding a phosphine ligand and cesium carbonate at the same time by taking Pd(PPh3)2Cl2 as a catalyst; adding strong base DBU or adding CuI as a cocatalyst to carry out sonagashira reaction, wherein the phosphine ligand is selected from tricyclohexyl phosphine (PCy3), tri-tert-butyl phosphine (PtBu3) or tri(funan-2-yl) phosphine (P(2-furyl)3). The method disclosed by the invention is complete in reaction, does not have or has extremely few diyne byproduct of alkyne coupling, and is easy to separate and purity.

The invention relates to a preparation method for 9-fluorenone and T type oligomeric phenylene skeleton compounds. The method includes: under the condition of 90-100DEG C, in a toluene solution, taking palladium acetate and tricyclohexylphosphine as the catalytic system, and adopting cesium carbonate as alkali, reacting o-dihalogenated aromatic hydrocarbon with arylboronic acid or aryl boric acid ester under CO atmosphere for 12h, thus obtaining a series of 9-fluorenone and T type oligomeric phenylene skeleton compounds. The method provided by the invention adopts simple, economical and easily available raw materials as the substrate, under the CO balloon pressure, palladium catalyzed carbonylation three-component cascade reaction is carried out to realize synthesis of 9-fluorenone compounds. Through bifunctionalization, Pi conjugated system expanded T type oligomeric phenylene skeleton compounds that are difficult to realize by previous methods can be constructed by one step, and the compounds have very great application prospects in pharmaceutical synthetic intermediates and organic photoelectric material science.

The invention provides a corona-resistant coating for a cable and a preparation method of the corona-resistant coating, and particularly relates to the technical field of cable materials. The coatingis prepared from the following raw materials: acrylic resin, ethanol, N,N'-diisopropylcarbodiimide, perfluoropolyether, resina draconis extract, mica, graphite type boron nitride, benzylidene-bis(triphenylphosphine)ruthenium dichloride, porphyrin compound, zirconium oxide and hexadecyltrimethylammonium bromide. The preparation method comprises the following steps: a, primary catalytic reaction; b,stabilizing treatment; c, secondary catalytic reaction; d, charging of nitrogen; and e, pre-coordination treatment. The coating disclosed by the invention can be well attached to a wire, does not generate air intermittence, has an air isolation effect and a highly conjugated structure, can play a role in preventing corona from multiple aspects, has corona resistance of 250 minutes, is not easy tocrack, has good insulativity and is not easy to break down. The method is stable in process, controllable in parameter, easy to repeat and suitable for large-scale production.

The invention discloses a method for production of tricyclohexylphosphine and belongs to the field of organic synthesis. The method comprises that triphenylphosphine oxide as an initial raw material undergoes a hydrogenation reaction in the presence of a catalyst to produce an intermediate tricyclohexylphosphine oxide; and the intermediate tricyclohexylphosphine oxide is reduced by KBH4-AlCl3 to form tricyclohexylphosphine. The method reduces a production cost, improves a product yield and is suitable for industrial production.

The invention discloses a method for synthesizing a second generation Grubbs catalyst, which relates to a catalyst, in particular to a metal carbine compound (H2IMes)(PCy3)(Cl)2Ru=CHPh(H2IMes is 1,3-di-(2,4,6-trimethylphenyl)imidazole alkyl, and PCy3 is tricyclohexyl phosphine) with favorable olefin double-decomposition catalytic activity, namely the second generation Grubbs catalyst. The method comprises the following step of reacting a zero valence ruthenium compound Ru(p-cymene)(COD)(p-cymene is paracymene, and COD is 1,5-cyclooctadiene) with PCy3, PhCHCL2 and a nitrogen heterocyclic carbine compound in toluene or other hydrocarbon solvents to obtain the second generation Grubbs catalyst. The invention has low cost and easy acquisition of used raw materials, simple and safe operation process, easy control and high yield and is particularly suitable for industrialized large production.

The invention discloses a preparation method of galaxolide, which comprises the following steps: carrying out methylene etherification reaction on hexamethyl indanol and a TEBBE reagent (CAS: 67719-69-1) under the action of a supported Pd catalyst, carrying out condensation cyclization to generate galaxolide, and carrying out continuous rectification to separate the product. The supported Pd catalyst is represented as Pd-X / Y, X is selected from triphenylphosphine, tributylphosphine, tricyclohexylphosphine, bis(diphenylphosphine) methane, 1, 2-bis(diphenylphosphine) ethane and 4, 5-bis(diphenylphosphin)-9,9-dimethyl xanthene, and Y is selected from carbon nanotubes, ordered mesoporous carbon, neutral alumina, silica, a molecular sieve and kaolin. The process provided by the invention avoidsthe problems of complex process, serious equipment corrosion, low safety, environmental friendliness and the like in the prior art, and the raw material conversion rate and the product selectivity can reach 93% or above.

The invention discloses a composite metal photocatalysis system which is represented by Ni-M-X-Y-Z, wherein M is selected from the group consisting of Al, Ag, Bi, Cd, Ge, Sb and Sn; x is selected fromthe group consisting of triphenylphosphine, triethylphosphine, tributylphosphine, tri-tert-butylphosphine and tricyclohexylphosphine; Y is selected from the group consisting of carbon nanorods, molecular sieves, ordered mesoporous carbon and silicon dioxide; Z is selected from the group consisting of diphenyl disulfide, dicumyl peroxide, hydrazine and 2,4-dinitrophenylhydrazine; the mass fractionof Ni is 10-20%; the mass fraction of M is 20-30%; the mass fraction of X is 20-40%; the mass fraction of Y is 15-40%,; and the mass fraction of Z is 10-30%. The catalytic system is used for preparing 1,1,2,3,3-pentamethylindane through free radical cycloaddition of alpha-methylstyrene and 2-methyl-2-butene, an conversion rate is larger than 90%, and selectivity is larger than 85%; and a catalystis stable and not prone to loss in the free radical cycloaddition reaction. A method provided by the invention is easy to operate and good in economic benefit.

The invention relates to the field of preparation of ruthenium-carbene catalysts, and discloses a preparation method of a ruthenium-carbene catalyst. The method comprises the following steps: (1) in the presence of an inert gas protective atmosphere and an organic solvent, performing a primary reaction on diazobenzyl and dihalotetra(triphenylphosphine)ruthenium at -20 DEG C to 0 DEG C for 15-60 minutes; and (2) in an inert gas protective atmosphere, performing a secondary reaction on the reaction product obtained in the step (1) and tricyclohexyl phosphine to obtain the di-tricyclohexyl phosphine-phenylethylene-dichlororuthenium complex. The method can be utilized to obtain the ruthenium-carbene catalyst at higher temperature within a shorter time at higher product yield, and is more suitable for implementing industrial production.

The invention relates to a preparation method of all-position replacement fluorene compounds obtained through halogen adjustment, control and synthesis. The method comprises the steps that at the temperature of 120-130 DEG C, halogen benzyl bromide reacts with arylboronic acid for 12 hours in a tetrahydrofuran solution under the atmosphere of inorganic base, additives and nitrogen where palladium acetate / tricyclohexylphosphine serves as a catalytic system, and a series of fluorene compounds are obtained. According to both methods, simple, economical and easily-obtained raw materials serve as the base materials, synthesis of the all-position replacement fluorene compounds is achieved through a palladium catalytic cascade reaction, and the compounds have a great application prospect in medicine synthesis midbodies and organic optoelectronic material science.

The invention relates to a preparation method of tricyclohexyl phosphine, which comprises the following steps: reacting a cyclohexyl Grignard reagent and phosphorus trihalide, dropwisely adding a saturated strongly-acidic weakly-alkaline inorganic salt water solution at low temperature to carry out quenching, adding tetrafluoroboric acid to prepare a salt, and resolving the salt with triethylamine to obtain the tricyclohexyl phosphine, wherein the cyclohexyl Grignard reagent is prepared by carrying out Grignard reaction on halogenated cyclohexane and magnesium metal under inert gas shielding. According to the invention, the product is subjected to after-treatment by a chemical process; the tetrafluoroboric acid firstly reacts with tricyclohexyl phosphine to form a salt to completely extract the tricyclohexyl phosphine from the reaction solution, and the salt is resolved with the triethylamine. The invention has very obvious beneficial effects, and greatly enhances the preparation yield; and the prepared product has the advantages of high purity, high quality and low preparation cost.

The invention provides a synthesis method of 2-methylene glutaronitrile. According to the method, tricyclohexylphosphine is taken as a catalyst; an acrylonitrile dimer is chemically catalyzed under the condition with a solvent or not; the dosage of the catalyst is 0.1-5.0 wt%; the reaction temperature is 50-90 DEG C; and the initial concentration of the acrylonitrile is 3.0-15.2 mol / L. Furthermore, the reaction product is purified in a distilling manner. The method is available in materials, mild in reaction condition, high in yield, good in selectivity, strong in atom economy, friendly to the environment and applicable to industrial production.

The invention provides a manganese (II) complex based on a tricyclohexylphosphine structure as well as a synthesis method and application thereof. Firstly, organic cations are obtained through ionization, and then the organic cations are combined with manganese bromide to form the ionic manganese (II) complex. The types of organic cations or the central configuration of metal manganese of the manganese (II) complex can be changed during synthesis, so that the photophysical properties of the manganese (II) complex can be regulated and controlled. As a cheap metal luminescent material with a wide prospect, the metal organic manganese halide material has a series of advantages of low cost, low toxicity, abundant reserves, excellent luminescent property and the like, and is applied to a plurality of fields such as information storage and encryption, organic electroluminescence, sensors, scintillators and the like.

The invention provides a synthesis method of cyclohexane dimethanol. The synthesis method comprises the following step: under the action of a catalyst, performing a hydroformylation reaction and a hydrogenation reaction on cyclohexene formaldehyde to obtain the cyclohexane dimethanol, wherein the catalyst comprises a cobalt compound and an organic tricyclohexylphosphine ligand; the cobalt compoundis preferably a hydrogenated polycarbonyl compound of cobalt. By adopting the synthesis method of the cyclohexane dimethanol, provided by the invention, the use of terephthalic acid and the like is avoided, the synthesis technology is simple, and the cost is low.

The invention discloses preparation of a loaded Grubbs catalyst and application of loaded Grubbs catalyst. The preparation is characterized in that: the catalyst is obtained by using the compound obtained by the amidation reaction of 3-3-ethenyl-4-isopropoxyphenyl-propionic acid as a loading precursor and then enabling the compound to carry out exchange complexation respectively with phenyl methylene-bistricyclohexylphosphine-dichlororuthenium or 1, 3-bis 2, 4, 6-trimethylphenyl-2-imidazolidinylidene-dichorobenzenemethylene-tricyclohexylphosphineruthenium; the catalyst is used for the olefin metathesis reaction of N,N-diallyl-4-methylbenzenesulfonamide and has quite strong catalytic activity. Compared with the prior art, the catalyst of the invention is simple in process and convenient in preparation, and can be recycled many times and keep excellent catalytic activity, thereby greatly reducing the heavy metal pollution caused by Grubbs type catalysts to the product of olefin metathesis reaction and developing a new way for green and environmentally-friendly organic synthetic chemistry.

A composition for use as a dental impression material including a polymerizable telechelic oligomer or polymer curable by ring-opening metathesis polymerization, a filler system, and a ruthenium carbene complex catalyst, whereby the catalyst initiates ring-opening metathesis polymerization of the composition. The invention includes a paste / paste system in which a base paste includes the polymerizable telechelic oligomer or polymer and a filler system and in which a catalyst paste includes the catalyst dissolved in an inert solvent and a filler system. The telechelic oligomer or polymer may be, for example, a polydimethylsiloxane end-functionalized with norbornyl groups. The catalyst may be, for example, a ruthenium carbene complex with a ligand having a basicity higher than tricyclohexylphosphine. The composition of the present invention exhibits reduced sensitivity to sulfur impurities.

The invention discloses a self-repairable photosensitive weld-retarding dry film. According to the invention, dicyclopentadiene and ethylidene norbornene are coated in microcapsule with the diameter of 1-10 [mu]m formed by urea-formaldehyde resin, the microcapsule is mixed with a carboxyl-containing alkali soluble polymer, a vinyl-containing unsaturated monomer or oligomer, a photoinitiator, an auxiliary agent, dicyclopentadiene, ethylidene norbornene, and bis(tricyclohexylphosphine)benzylidine ruthenium dichloride, a support is coated by a mixture and then dried; the upper layer is applied with a polymer cover membrane, and then the self-repairable photosensitive weld-retarding dry film is prepared. After a self-repairable material is introduced into the weld-retarding dry film, the weld-retarding dry film can realize self repairing when the defects of crack and cavity are generated, anti-welding performance and insulating property of a circuit board are guaranteed, and the usage life of the circuit board is greatly prolonged.