20 results about "Alkynylation" patented technology

This invention provides a PMMA-PCL-based composite solid electrolyte, its preparation method, and its applications. The composite solid electrolyte comprises the following components: polymethyl methacrylate, polycaprolactone, lithium salt, active lithium-containing filler, and an unsaturated alkynyl compound with photoinduced secondary self-enhancing properties. This invention promotes supramolecular homogeneous integration within the electrolyte through magnetic field-microwave coupling and, for the first time, introduces an unsaturated alkynyl compound with photoinduced secondary self-enhancing properties to anchor solvent molecules and anions, thereby regulating the local coordination environment of lithium ions at the interface to improve lithium-ion transport and interfacial stability of the PMMA-PCL-based composite solid electrolyte at room temperature. This results in the PMMA-PCL-based composite solid electrolyte provided by this invention exhibiting excellent room-temperature performance and significantly improving the performance of symmetric cells at 0.1 mA cm⁻¹. ‑1 The time it takes for the current density to allow for stable cycling.

The invention relates to a method for decarbonylation alkynylation of ketone, which comprises the following step: in an inert solvent, under the action of a metal catalyst and a ligand, carrying out decarbonylation-reduction coupling reaction on a ketone compound and alkynyl chloride to obtain an alkyne compound. The alkyne is synthesized under the strategy of nickel catalysis, and the method has the advantages of easily available raw materials, simple operation and mild conditions, has very good theoretical guidance significance and practical application value, and conforms to the sustainable green chemistry concept.

The invention belongs to the technical field of complex enyne preparation, and particularly relates to a method for synthesizing complex enyne through selective alpha / beta C-H alkynylation of aryl olefin and application of the complex enyne, and the method comprises the following steps: under relatively mild conditions, adopting a transition metal salt catalyst, enabling the aryl olefin and an alkynylation reagent to be subjected to selective alpha / beta C-H alkynylation reaction, and obtaining the complex enyne through selective alpha / beta C-H alkynylation. Complex alkyne is prepared; wherein the molar ratio of the aryl olefin to the alkynylation reagent to the transition metal salt catalyst to the additive is 1 to (1.5 to 2.5) to (0.05 to 0.15) to (1.5 to 3.0); according to the method for synthesizing the complex alkyne through selective alpha / beta C-H alkynylation of the aryl olefin and the application of the complex alkyne, the synthesis efficiency is high, the E / Z selectivity is excellent, the method is environmentally friendly, the production environmental protection pressure is small, the substrate application range of the method is wide, and individual substrates can be used for preparing luminescent layer materials of photoelectric devices or preparing anti-counterfeit labels and the like.

This invention relates to the field of organic synthesis technology, and in particular to a method for synthesizing alkynyl compounds based on mechanical ball milling. An ether compound is mixed with a compound of formula V, sodium iodide, and ethyl acetate, and then subjected to a ball milling reaction to obtain the alkynyl compound. The ball milling reaction conditions include a vibration frequency of 30 Hz and a vibration time of 30 min. This invention provides the first method to apply a mechanical strategy to the generation of alkynyl free radicals and the subsequent selenization reaction. Through ball milling-induced σ-hole sulfur bond SET, alkynyl sulfonium salts generate alkynyl free radicals and synthesize alkynyl selenides. Compared with existing technologies, the method for generating alkynyl free radicals described in this invention does not require metal catalysts or ultraviolet excitation, achieves high yields of alkynyl selenides, and features simple operation and mild reaction conditions.

The application discloses a transition metal-free method for preparing o-iodophenyl acetylide, which uses o-dihalobenzene and terminal alkyne as raw materials, and reacts to obtain o-iodophenyl acetylide in the presence of alkali metal hydride; preferably, the reaction is carried out in a solvent. Specifically, the alkali metal hydride is added into the solvent, then the terminal alkyne compound is added, stirred for 5 min, and then the o-dihalobenzene is added, and the reaction is carried out at 0-60 DEG C to obtain the alkylation product o-iodophenyl acetylide. The method is simple in operation, mild in reaction condition, and can be easily scaled up, and does not need any metal additive or anhydrous condition.

The invention discloses a synthesis method of a 2-alkynyl-3-ester pyrrole compound, which comprises the following steps: by taking a pyrrole derivative and (bromoethynyl) triisopropyl silane as raw materials, under the conditions of a silver additive and alkali, catalyzing a pyrrole C2 site direct alkynylation reaction by using a ruthenium catalyst to prepare the 2-alkynyl-3-ester pyrrole compound. The method is based on a precise C-H activation strategy of a ruthenium catalyst, and through reasonable matching of the ruthenium catalyst, a silver salt additive and an alkali system, the activity of a metal center can be effectively regulated and controlled, so that the metal center selectively recognizes a pyrrole C2 site and precise and directional introduction of alkynyl is realized, thereby overcoming challenges such as site competition and catalytic circulation blocking caused by an electronic effect. In a word, the alkynylation system established by the invention is simple and convenient to operate and good in repeatability, provides a reliable technical approach for rapid preparation of the 2-alkynyl-3-ester pyrrole compound, expands a new synthesis thought for construction of drug molecules, functional materials and organic photoelectric structural units, and has important application value and popularization prospect.

The invention discloses a method for synthesizing a benzofuran derivative through copper-catalyzed alkynylation reaction, and relates to the technical field of organic synthetic chemistry and medicinal chemistry. According to the method, halogenated anisole and terminal alkyne are used as raw materials, under the combined action of a copper catalyst and alkali, ethanol is used as a green solvent, an aryne intermediate is generated in situ through a Sonogashira coupling reaction, then an electrophilic reagent R-Se-X1 is directly added to induce cyclization without separation and purification, and a benzofuran skeleton is efficiently constructed. Compared with a traditional palladium catalysis system, the method has the advantages that the copper catalyst which is low in cost and easy to obtain is adopted, the problems of high cost and difficult recovery of precious metal (such as palladium) are solved, meanwhile, the use of cocatalysts of heavy metal (such as lead and antimony) is eliminated, and the economical efficiency and the environmental protection property of the process are remarkably improved. In addition, the reaction for synthesizing the aryne intermediate does not need inert gas protection, and the reaction conditions (heating and room temperature) are mild. In addition, the method provided by the invention also has excellent substrate universality.

The invention discloses the crystal form, preparation method and application of an alkynyl compound, its salt and solvent compound. The invention specifically discloses 3-((1H-pyrazolo[3,4-b]pyridin-5-yl)ethynyl)-4-methyl-N-(4-((4-methylpiperazine-1-yl)methyl)-3-(trifluoromethyl)phenyl) benzamide crystal form I and 3-((1H-pyrazolo [3,4-b]pyridin-5-yl)ethynyl)-4-methyl-N-(4-((4-methylpiperazine-1-yl)methyl)-3-(trifluoromethyl)phenyl) benzamide fumarate crystal form II. The crystal form of the invention has good stability and has important value for drug optimization and development.

The invention discloses a high-performance polymer interpenetrating network and a preparation method thereof. The preparation method comprises the following steps: 1) mixing alkynylated polyethylene glycol, dimethyl ethylenediamine, trimethylolpropane tripropiolate and a monodentate ligand in a first solvent for reaction, adding palladium acetate and the tridentate ligand for coordination reaction after the reaction is finished, and removing the first solvent after the coordination reaction is finished to obtain a polyethylene glycol network; and 2) in the presence or absence of a catalyst, mixing the polyethylene glycol network, polyol, a chain extender, polyisocyanate and a cross-linking agent to react to obtain a polyethylene glycol-polyurethane polymer interpenetrating network, and curing to obtain the high-performance polymer interpenetrating network. According to the invention, the mechanical property and energy absorption capacity of polyurethane and polyethylene glycol can be enhanced, so that the material can bear higher stress level, the toughness of the material is improved, and the maximum extensibility and plastic deformation capacity of the material are improved while the original strength of a polymer is maintained.

The invention relates to the technical field of high polymer materials, in particular to a wear-resistant PEEK composite material and a preparation method thereof.The preparation method comprises the steps that phenylethynyl phthalic anhydride is added into polyether-ether-ketone powder for evaporation end-capping treatment, end-capped polyether-ether-ketone with an alkynylated large end and a small end is formed, and end-capped polyether-ether-ketone with the alkynylated large end and the small end is prepared; dispersing the mixed filler particles in a mixed solution containing a silane coupling agent, stirring, and carrying out melt mixing treatment on the stirred composite filler and terminated polyether-ether-ketone to obtain a composite melt; carrying out hot pressing on the composite melt to form a crystal structure, and carrying out thermal cycle diffusion treatment on the crystal structure to obtain a heat treatment product comprising an interface diffusion layer; and performing scanning treatment on the heat treatment product based on pulse laser to melt the polyether-ether-ketone on the surface layer and activate the interface diffusion layer to form the wear-resistant composite material comprising the wear-resistant coating. The technical problems that in the prior art, a wear-resistant coating is weak in interface bonding force with a base body and prone to being stripped too early are solved, and the wear rate is greatly reduced compared with the prior art.

Methods, compositions, and kits are provided for synthesizing bioactive chromane, the method including: constructing a tertiary ether stereocenter enantioselectively by catalyzed alkynylation of a substituted chromenone to obtain a chromanone; reducing alkyne and ketone in the chromanone to obtain a chroman; and converting ester to methyl group thereby obtaining chromane.

The invention discloses a preparation method of an NHC-boronized alkyne compound, which comprises the following specific preparation process: taking an ethynyl benzoxazolinone compound and an N-heterocyclic carbene borane compound as reaction raw materials, 4-CzIPN as a photocatalyst, Cs2CO3 as alkali and acetonitrile as a solvent, and reacting under blue light LED irradiation and nitrogen atmosphere to obtain the NHC-boronized alkyne compound. And finally, the target product NHC-boronized alkyne compound is prepared. Through visible light catalysis, the reaction condition is mild, the operation is simple and convenient, N-heterocyclic carbene borane which is easy to synthesize is used as a boron source, ethynyl benzoxazolinone is used as an alkynylation reagent, and various NHC-boronized alkyne compounds can be efficiently synthesized.

[Problem]To provide an alkenyl phosphorus compound.[Means to Solve the Problem]The method for manufacturing an alkenyl phosphorus compound according to the present invention is a method in which a specific phosphorus compound and a specific alkynyl compound are reacted in the presence of a transition metal complex and a Lewis acid, thereby giving an alkenyl phosphorus compound.

The invention belongs to the technical field of sealants, and particularly discloses a curing stabilizer, a sealant based on the curing stabilizer and a preparation method.The curing stabilizer is prepared from, by weight, 100 parts of N-(4-methoxybenzyl) hydroxylamine; 20-80 parts of an aldehyde compound; 30 to 50 parts of triethylamine; 300 to 500 parts of dichloromethane; 12 to 40 parts of a terminal alkynyl compound; 190 to 300 parts of acetonitrile; 10 to 20 parts of water; 50 to 150 parts of ceric ammonium nitrate; wherein the aldehyde compound is at least one of formaldehyde, acetaldehyde and benzaldehyde; the alkynyl-terminated compound is at least one of phenylacetylene and trimethylsilylacetylene. The curing stabilizer disclosed by the invention has a relatively good application value in prolonging the storage period of the sealant and increasing the curing speed.

This invention discloses a gold / silver catalyzed method for synthesizing 3-alkynylpyrrole compounds, belonging to the field of organic synthesis technology. The method uses enamine compounds and alkynyl high-valent iodine(III) reagents as raw materials, in acetonitrile solvent, with Ph3PAuNTf2 (5 mol%) and AgPF6 (5 mol%) as catalysts, and 1,10-phenanthroline (20 mol%) as a ligand, via a tandem C(sp... 2 The α-H-ynylation / N-ynylation reaction enables the one-step construction of a multi-substituted pyrrole skeleton. This synthetic method features mild reaction conditions, simple operation, a wide range of applicable substrates, good compatibility with various functional groups, and the ability to achieve gram-scale reactions, making it of significant application value in the fields of medicinal chemistry and functional materials.

The application discloses a synthesis method of a functionalized carbon glycoside, and belongs to the technical field of organic synthesis. The application takes a coupling reagent (aryl bromide, alkenyl bromide, alkenyl geminal difluoride, alkynyl bromide, electron-deficient olefin) and a glycoside as substrates, is catalyzed by a photocatalyst, or is cooperatively catalyzed by a photocatalyst and a metal catalyst, and is completely reacted under the irradiation of purple light to obtain a functionalized (arylated, alkenylated, alkenyl monofluorinated, alkynylated and alkylated) carbon glycoside. The application realizes the stereoselective functionalization reaction of a C(sp 3 )‑H bond of the glycoside by using the strategy of photocatalysis or light-metal cooperative catalysis, the method has the advantages of mild conditions, wide substrate adaptability, low cost, high atom utilization rate and economic steps, and the synthesized functionalized carbon glycoside can realize the synthesis of various natural products and commercially available drugs through subsequent conversion, and has great synthetic value.

The application belongs to the technical field of flame retardants, and particularly relates to a nitrogen-phosphorus modified lignin-based flame retardant, a preparation method and application thereof, and the preparation method of the nitrogen-phosphorus modified lignin-based flame retardant, which comprises the following steps: adding an alkynylating reagent and an activating agent into an organic solution of lignin, heating and stirring, performing an alkynylating modification reaction to obtain alkynylated lignin; mixing the alkynylated lignin with a phosphating reagent in an organic solvent, heating and stirring, and performing a phosphating reaction to obtain phosphated lignin; mixing the phosphated lignin, an azide and a composite catalyst in an organic solvent in a nitrogen atmosphere, heating and stirring, and performing an azidation modification to obtain the flame retardant. The lignin is used as a main raw material, and high-value utilization of the lignin and improvement of the flame retardant performance of the composite material are realized.

The invention provides insulating lubricating oil for an electric compressor of a new energy automobile and a preparation method thereof, and belongs to the technical field of special lubricating oil. The preparation method comprises the following steps: carrying out alkynylation pre-activation on a small amount of polyol ester (POE) base oil, and then covalently linking the activated POE and poly-alpha olefin (PAO) base oil by using a bifunctional crosslinking agent containing furan and maleimide groups by adopting a series distribution process of a copper-catalyzed azide-alkyne cycloaddition reaction (CuACC) and a photo-initiated enol-sulfur reaction. Finally, a dynamic network structure is formed through a reversible cycloaddition reaction between furan and a maleimide group, a functional additive is added, and the insulating lubricating oil capable of self-adjusting the state according to different working conditions of the compressor is obtained. The lubricating oil composition has excellent electrical insulating property, excellent working condition self-adaptive rheological property and high chemical stability and material compatibility, and meets the strict requirements of the new energy automobile electric compressor on lubrication and insulation.

The invention discloses a preparation method and application of a dehydrorotaxene derivative. According to the method, acetylenic bonds are introduced into a double-bond conjugated system through olefin hydrocarbon activation alkynylation reaction, then ring closing reaction is completed under the Glaser-Hay coupling condition, so that synthesis of dehydrorotaxene is achieved, and the problems that dehydrorotaxene synthesis steps are tedious, and atom economy is poor are solved. The method for synthesizing dehydrorotaxene is high in atom utilization rate and good in functional group compatibility. The compound prepared by the invention has certain adsorption capacity on iodine simple substances, is physical adsorption, and has application potential of adsorbing radioactive iodine in nuclear waste.

This invention belongs to the field of chemical synthesis technology, specifically relating to a method for the direct-directed nickel-catalyzed Markovnikov hydroynkylation of amino groups to synthesize γ-ynylamines from non-activated olefins. The method includes mixing ethylene glycol dimethyl ether dibromide, ethylenediamine ligands, 3-en-1 amine compounds, potassium benzoate, trimethoxysilane, ynyl bromide, and an ether solvent. The resulting mixture undergoes a Markovnikov hydroynkylation reaction to yield γ-ynylamine compounds. This reaction utilizes inexpensive and readily available nickel catalysts (such as NiBr2·DME) and hydroxyl sources (such as (MeO)3SiH) under mild conditions, and is compatible with tertiary cyclic / acyclic amines and secondary alkyl / aryl amine substrates, as well as aryl, alkyl, and silyl-substituted ynkylation reagents, achieving a broad substrate applicability. Furthermore, this preparation method exhibits mild reaction conditions, good regioselectivity, and low cost, demonstrating excellent industrialization potential.