41 results about "Enamine" patented technology

The invention relates to a method for synthesizing an iodo-pyridine compound from N-propargyl enaminone, which comprises the following steps: by taking N-propargyl enaminone as a raw material, DMF (Dimethyl Formamide) as a reaction solvent and copper acetate and N-iodosuccinimide as accelerators, carrying out intramolecular coupling reaction at 60 DEG C to synthesize the iodo-pyridine compound. The method for directly synthesizing the pyridine heterocyclic compound through the intramolecular coupling reaction of the N-propargyl enaminone under the non-alkaline condition is disclosed for the first time, reaction substrates are not limited to benzene rings on alkynyl, the application range of the reaction is greatly expanded, and the method has the advantages of being wide in substrate range, strong in functional group application range, mild in reaction condition, easy to operate, safe, high in yield and the like. And raw materials are cheap.

The invention discloses a perfluoroalkyl-substituted pyrimido [1, 2-b] indazole ketone compound and a preparation method thereof, and belongs to the technical field of compounds containing two or more heterocyclic rings. Comprising the following steps: with enaminone, a perfluoroalkane compound and aminoindazole as raw materials, carrying out a reaction under blue light irradiation in the presence of an organic solvent and alkali to prepare the perfluoroalkyl-substituted pyrimido [1, 2-b] indazole ketone compound; according to the invention, through visible light mediated dehalogenation and cyclization free radical addition, high-yield synthesis of the perfluoroalkyl substituted pyrimido [1, 2-b] indazole ketone compound is realized; the prepared perfluoroalkyl-substituted pyrimido [1, 2-b] indazolone compound has excellent antibacterial activity, can be used for preparing antibacterial drugs, and has outstanding industrial application value.

The application discloses a tetravalent platinum ester alkyne complex, a degradable high polymer, a nanomicelle and a preparation method and application thereof; the structural formula of the tetravalent platinum ester alkyne complex is shown as formula (I); the preparation method of the degradable high polymer is as follows: the tetravalent platinum ester alkyne complex is prepared first; then the obtained tetravalent platinum ester alkyne complex and diamine and monomethyl ether polyethylene glycol mPEG-NH2 are clicked to obtain a triblock high polymer. The nanomicelle of the degradable high polymer is also disclosed. The tetravalent platinum ester alkyne complex disclosed by the application can specifically respond to reducing substances in a tumor microenvironment, and the enamine ester structure generated by the reaction of the tetravalent platinum ester alkyne complex with diamine also has the property of responding to an acidic environment; the high polymer has mild and simple preparation conditions, the molecular weight can reach 35200, and the platinum drug loading capacity is as high as 33.91%; the nanomicelle can efficiently degrade and release anticancer active drugs in the tumor microenvironment, and has high antitumor activity and low cytotoxicity.

The invention provides preparation and application of a benzophenone ketone enamine visible light initiator. The benzophenone keto enamine is a compound with a structural formula as shown in a formula (I). The benzophenone keto enamine provided by the invention is an LED visible light initiator, can be used as a single-component photoinitiator and can also be compounded with other substances for initiation, and when the benzophenone keto enamine provided by the invention is used as the photoinitiator, the initiation effect is good, and the benzophenone keto enamine can be adapted to an LED light source of 405-470 nm.

The invention provides a method for catalytically synthesizing 7-amino-3-oxabicyclo [3.3. 1] nonyl-6-ene-1-ol by using rare earth, which comprises the following steps of: adding a catalyst and a catalyst, according to the preparation method, rare earth trifluoromethanesulfonate is taken as a catalyst, 6-alkoxy-2, 6-dihydropyran-3-ketone and enamine compounds are taken as raw materials, and the 7-amino-3-oxabicyclo [3.3. 1] nonyl-6-ene-1-ol is prepared by catalyzing (3 + 3) cyclization reaction. The synthesis method provided by the invention is simple in reaction raw material synthesis, low in rare earth salt price, easy in experimental operation and suitable for large-scale preparation. The obtained compound can be applied to the fields of organic synthesis, drug synthesis, organic materials and the like.

This invention discloses a method for synthesizing a tenapano hydrochloride intermediate. The synthesis method includes the following steps: (1) condensing the compound 3-bromophenylacetaldehyde and the compound N-methyl-(2,4-dichlorophenyl)methylamine under dehydration conditions to obtain an enamine intermediate; (2) subjecting the enamine intermediate to an intramolecular cyclization reaction in the presence of an acid catalyst to obtain the tenapano hydrochloride intermediate 4-(3-bromophenyl)-6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinoline. The synthetic route provided by this invention requires only two steps to construct the key framework, and has the advantages of short reaction steps, high overall yield, and no need to use highly toxic liquid bromine. This process has high atom economy, reduces the emission of waste gas, wastewater, and solid waste, and is suitable for large-scale industrial production under mild conditions.

This invention relates to the field of pharmaceutical intermediates, and in particular to a method for synthesizing chiral indane. The method uses indane as a raw material, synthesizes an oxime, then an enamine, and subsequently synthesizes the trans-chiral indane via an asymmetric hydrogenation reaction using a ruthenium chiral bisphosphine catalyst, achieving high yield and high stereoselectivity. The advantages of this invention are: in the asymmetric hydrogenation reaction of the enamine, the trans-chiral indane is obtained with a content greater than 97%, an ee of 95%, and a yield greater than 90%; the catalyst is readily available; the operation is simple; the raw materials are readily available; there is minimal pollution from waste; and energy consumption is low, making it suitable for industrial production.

The invention provides a method for preparing an acetamidine solution and co-producing enamine from sodium and acetamidine hydrochloride, and relates to the technical field of organic synthesis.The method comprises the following steps that sodium and acetamidine hydrochloride are subjected to a free reaction, byproduct salt is removed, a mixed solution of acetamidine and an intermediate is obtained, the mixed solution is taken to be layered, and enamine is obtained; the supernatant is acetamidine liquid, and the subnatant is an intermediate; and carrying out condensation reaction on the intermediate and o-chloroaniline to obtain enamine. The invention solves the problems of tedious process and high energy consumption of the existing acetamidine hydrochloride dissociation process, and achieves the technical effects of reduced raw and auxiliary materials, low cost, simple process and low energy consumption.

The invention discloses an aliphatic beta-keto-enamine bond covalent organic framework material based on pyrrolidine catalytic synthesis, the skeleton structure of the covalent organic framework material comprises a beta-keto-enamine bond formed by condensation reaction of 1, 3, 5-trialdehyde phloroglucinol and an aliphatic ammonia monomer, and the preparation method comprises the following steps: adding 1, 3, 5-trialdehyde phloroglucinol and an aliphatic amine monomer into a reaction kettle, and reacting to obtain the covalent organic framework material. The preparation method comprises the following steps: mixing 1, 3, 5-trialdehyde phloroglucinol, an aliphatic ammonia monomer, a solvent and a catalyst for reaction, washing and drying to obtain the covalent organic framework material containing the beta keto-enamine bond. According to the invention, pyrrolidine is adopted as a high-efficiency catalyst and is matched with a green mixed solvent system with specific composition, so that ordered connection of flexible aliphatic ammonia monomers is effectively guided, the problem that low polymers are easy to generate under the catalysis of traditional acetic acid is overcome, and the crystallization quality of the material is remarkably improved.

The invention provides a method for catalytically synthesizing 7-oxa-2-azabicyclo [3.3. 1] nonyl-3-ene-1-ol by using rare earth, which comprises the following steps of: adding a catalyst and a catalyst, according to the preparation method of the 7-oxa-2-azabicyclo [3.3. 1] nonyl-3-ene-1-ol, rare earth trifluoromethanesulfonate is taken as a catalyst, 6-alkoxy-2, 6-dihydropyran-3-ketone and enamine compounds are taken as raw materials, and the preparation of the 7-oxa-2-azabicyclo [3.3. 1] nonyl-3-ene-1-ol is realized. The method is simple in reaction raw material synthesis, simple in experimental operation and suitable for large-scale preparation. The obtained compound can be applied to the fields of organic synthesis, drug synthesis and the like.

The application discloses a kind of by density functional theory reveals the calculation method of micro-mechanism and selectivity source of palladium catalysis olefin amine 1,2-diarylation reaction, belong to the intersection technical field of organic synthesis and computational chemistry. Including constructing molecular structure;The configuration optimization and calculation are carried out to molecular structure, obtain thermodynamic data;The geometric configuration of intermediate and transition state in each step is calculated, the change of gibbs free energy is obtained, the connection relationship of transition state and corresponding reactant, product is determined;According to thermodynamic data and connection relationship, reaction path diagram is drawn, and reaction mechanism is determined;According to reaction mechanism, the step of determining the selectivity of reaction region, enantioselectivity and chemical selectivity is determined, and selectivity control strategy is analyzed and output. By simulation, the key intermediate and transition state structure of each element step of reaction is determined, the reaction energy barrier of each element step is quantified, the transition state action mechanism determining the selectivity of reaction region, enantioselectivity and chemical selectivity is analyzed in depth, to provide theoretical guidance for the design of high-efficiency catalyst and the optimization of reaction condition.

This invention provides a clay stabilizer and its preparation method. First, a low molecular weight polymer is obtained by polymerizing acrylate, acrylamide, and dimethyl diallyl ammonium chloride in an aqueous solution. Then, an amidation reaction is carried out with enamine or alkyl diamine to obtain the clay stabilizer. This clay stabilizer has the advantages of good anti-swelling effect and long-lasting effect, effectively preventing clay particle migration, good temperature resistance, not increasing formation water salinity, and increasing formation permeability. The anti-swelling rate is ≥95%, the anti-swelling rate after aging at 350℃ is ≥90%, the water washing resistance rate is ≥97%, the core permeability recovery rate is ≥85%, and the core permeability retention rate is ≥90%.

The invention discloses a composition, a thin film and a photoelectric device, the composition comprises at least one P-type organic compound and at least one enamine compound, the enamine compound can promote molecular crosslinking of the P-type organic compound, so that the composition has good hole transport performance, and the composition can be applied to preparation of the photoelectric device. And the hole mobility of the photoelectric device is improved, so that the device efficiency and the device service life of the photoelectric device are improved.

This invention discloses indole-fused hydrogenated morpholino compounds, their preparation methods, and applications, belonging to the technical fields of fluorescent materials and antitumor compounds. Using enamine ketones and amines as reaction substrates, a series of indole-fused hydrogenated morpholino compounds with different substituents were synthesized in highly polar solvents via the Stork enamine reaction and intramolecular acylation reaction. These compounds exhibit fluorescence wavelengths in the range of 430-700 nm and show certain inhibitory activity against lung cancer A549, breast cancer MDA-MB-231, colon cancer HCT116, liver cancer HepG2, and prostate cancer DU145, providing more options for the preparation of tumor drugs.

This application provides a ketene-enamine covalent organic framework thin film, its preparation method, and its application. The preparation method includes: mixing an aldehyde monomer with an acetic acid solution to obtain an aldehyde monomer solution; mixing an amine monomer with water to obtain an amine monomer solution; mixing the amine monomer solution and the aldehyde monomer solution and then performing a condensation reaction to obtain a first mixture containing an imine intermediate; mixing the first mixture with water to obtain a second mixture; centrifuging the second mixture to obtain a precursor solution containing the imine intermediate; and performing a film-forming treatment on the precursor solution, during which the imine intermediate reacts to form a ketene-enamine material, thereby obtaining the ketene-enamine covalent organic framework thin film. This invention can shorten the film preparation cycle and obtain ketene-enamine covalent organic framework thin films with high mechanical strength and good stability.

Disclosed are degradable tough hydrogels using enamine N-oxide based crosslinkers. Also disclosed are methods of making and using the degradable tough hydrogels.

The application discloses a kind of continuous hydrogenation reduction synthesis 1-(2-aminoethyl) pyrrolidine method in the technical field of pharmaceutical synthesis, which takes aminoacetaldehyde acetal as raw material, by adding acid catalyst in the reaction system, in-situ generation aminoacetaldehyde, further and pyrrolidine form enamine, continuous hydrogenation reduction reaction in microreactor, high yield 1-(2-aminoethyl) pyrrolidine is obtained.The application has the advantages of low raw material cost, short reaction time, high product purity and yield, is friendly to environment, reaches the requirement of green chemical process.

A method for preparing diethylenetriamine crosslinked liquid polybutadiene rubber is disclosed. The crosslinked rubber prepared by this invention uses polybutadiene as the main chain and diethylenetriamine as the crosslinking agent. The primary amine groups on the diethylenetriamine molecule react with aldehyde groups to form imine bonds, and the secondary amine groups react with aldehyde groups to form enamines. The preparation process involves: firstly, oxidatively cracking cis-butadiene rubber to prepare aldehyde-terminated polybutadiene; then, adding diethylenetriamine at a mass ratio of 0.03–0.1:1 to the aldehyde-terminated polybutadiene, and preparing the crosslinked rubber using the above reaction. The mixture of diethylenetriamine and aldehyde-terminated polybutadiene can be crosslinked at room temperature, exhibiting low energy consumption and high reactivity, overcoming the problems of complex crosslinking processes or high energy consumption caused by traditional crosslinking rubber using sulfur or peroxides. This rubber possesses self-healing and reusable properties, overcoming the problems of traditional crosslinked rubbers being non-self-healing and non-recyclable.

This invention relates to the field of hygiene products, providing an antibacterial absorbent core and its preparation method, solving the problem that existing antibacterial absorbent cores lack anticoagulant function and that Ag is added during coating. + This facilitates its migration into the human body or the addition of Ag. + The method leads to a relatively poor antibacterial effect; the antibacterial absorbent core includes a lower nonwoven fabric layer, a SAP and modified PET fiber mixture layer, an sizing layer and an upper nonwoven fabric layer stacked from bottom to top; wherein the SAP and modified PET fiber mixture layer is obtained by mixing SAP and modified PET fibers and then negative pressure adsorption, conveying and molding, and the modified PET fibers include the following raw materials: acetone, anhydrous ethanol, PET fibers, sodium periodate, dopamine hydrochloride, N,N-dimethylformamide, propylene glycol methyl ether, silver ammonia solution, azodiol enamine, hydrochloric acid, N,N-dimethylformamide and deionized water.

The invention discloses a synthesis method of an enamine compound and a recycling method of raw materials, and belongs to the technical field of pesticide chemical industry. According to the method, ethyl trifluoroacetoacetate is used as a raw material, substituted phenylacetic acid ammonium is used as an amination reagent, 3-amino-4, 4, 4-ethyl trifluorocrotonate is prepared through a reflux water diversion reaction in a specific organic solvent, and efficient recovery of the amination reagent is achieved through ammonia water mediation. Water generated by reaction is removed in time through reflux water diversion, raw material ester hydrolysis is effectively inhibited, and the yield of enamine is larger than or equal to 98%; and in the recovery process, sublimation is avoided by utilizing the high-boiling-point characteristic of substituted phenylammonium acetate, the problem of condenser blockage is solved, the recovery yield is greater than or equal to 99%, direct application can be realized, the cost is remarkably reduced, and green chemical requirements are met.

The application relates to the technical field of organic synthesis, and provides a synthesis method of chiral allylamine and application thereof, which takes isoegual and chiral tert-butylsulfonamide as initial raw materials, synthesizes an enamine intermediate M1, adopts a silyl ether protecting group to protect a phenolic hydroxyl group to obtain an intermediate M2, then carries out a Grignard reaction on the intermediate M2 to obtain an intermediate M3, then removes a sulfinyl group from the intermediate M3 to obtain an intermediate M4, and then acetylates to obtain an intermediate M5, and finally removes a silyl ether protecting group from the intermediate M5 to obtain the chiral allylamine. The synthesis method can reduce the preparation cost of the chiral allylamine, is beneficial to industrialized production, optimizes stereoselectivity, and omits a chiral resolution step, and the chiral allylamine can be used for synthesizing colchicine.

The invention discloses an irradiation-resistant vapor phase corrosion inhibitor and a preparation method and application thereof, and relates to the field of metal protection in special environments, and the vapor phase corrosion inhibitor comprises the following components in parts by weight: 20-50 parts of a main corrosion inhibitor, 10-30 parts of a synergistic corrosion inhibitor, 5-15 parts of a metal deactivator, 10-25 parts of an irradiation stabilizer and the balance of a carrier and a dispersant. The main corrosion inhibitor is prepared through efficient enamine synthesis reaction of aromatic aldehyde or aromatic aldehyde compounds and morpholine under the catalysis of organic acid. According to the vapor phase corrosion inhibitor, through the synergistic effect of all the components, the vapor phase corrosion inhibitor exerts excellent vapor phase anti-rust performance, meanwhile, the molecular structure of the vapor phase corrosion inhibitor can effectively resist damage of high-energy irradiation such as gamma rays, and long-term stability is kept. The product can be prepared into various forms such as powder, tablets and the like, and is specially used for protecting metal products in strong irradiation environments such as nuclear power stations, nuclear waste treatment facilities and the like from being corroded.

This invention belongs to the field of organic synthesis technology, specifically relating to a method for preparing racemic nicotine and a method for resolving levorotatory nicotine. The method for preparing racemic nicotine includes the following steps: First, a Grignard reagent is prepared using 3-bromopyridine and magnesium as raw materials; then, N-methylpyrrolidone is added to the Grignard reagent for a condensation reaction. After the reaction, an enamine intermediate is obtained, followed by the addition of an acid to obtain an ammonium salt; finally, the obtained ammonium salt is reacted under the action of a reducing agent to prepare racemic nicotine. Levorotatory nicotine is obtained by resolving and recrystallizing racemic nicotine with L-(-)-dibenzoyl tartaric acid in a mixed solvent of methanol and isopropanol through two stages. The method for preparing racemic nicotine using this invention uses inexpensive starting materials, has mild reaction conditions, and yields a high product yield. Furthermore, the method for resolving levorotatory nicotine in this invention involves fewer chiral resolution steps, achieves good resolution, and is suitable for industrial-scale production.

The invention belongs to the technical field of photocatalysis, and particularly relates to a preparation method and application of a multifunctional sulfur-zinc-cadmium photocatalyst. The method comprises the following steps: preparing a sulfur-zinc-cadmium crystal nucleus through a liquid-phase ion exchange method, promoting regrowth of the sulfur-zinc-cadmium crystal nucleus through a molten salt calcination method to obtain a sulfur-zinc-cadmium photocatalyst, and carrying out sulfur ion modification on the surface of the sulfur-zinc-cadmium photocatalyst through a coprecipitation method to obtain sulfur-zinc-cadmium with a sulfur-rich surface. And finally, selectively depositing Pd nano-particles on the high-index crystal face of the sulfur-zinc-cadmium with the sulfur-rich surface through photochemical reduction to obtain the multifunctional sulfur-zinc-cadmium photocatalyst. The catalyst can be used for a reaction system for preparing N-benzylidenebutylamine through benzylamine coupling, preparing hydrogenated benzoin through benzyl alcohol coupling, preparing 2-hydroxymethyl pyrazine through 2-formic acid pyrazine reduction and preparing benzaldehyde and other template micromolecular aromatic compounds through benzyl alcohol oxidation. The catalyst is simple in preparation method and wide in raw material source, can drive reactions such as coupling, reduction and oxidation of small molecular aromatic compounds, and has industrial application prospects.

The present invention provides a method for preparing a chiral 4-aryl-β-amino acid derivative. The preparation method comprises hydrogenating an enamine compound having a structure as shown in Formula III in an organic solvent in the presence of a catalyst containing a transition metal and BIBOPs. The preparation method of the present invention uses a small amount of a selected asymmetric catalyst, and has a simple operation, mild reaction conditions, a high yield, a high stereoselectivity, and better industrial application and economic values.

The invention discloses a preparation method of sitagliptin, and belongs to the technical field of medicine synthesis. The method takes decarboxylation condensation and asymmetric reduction as core reaction steps, and comprises the following steps: firstly, decarboxylation condensation is performed on a cyano compound I and a compound II in an organic solvent A under the action of metal salt and alkali to generate an enamine intermediate III; the intermediate III is subjected to asymmetric reduction in an organic solvent B through a reducing agent, a reaction accelerant and a chiral catalyst, and sitagliptin is obtained. By optimizing raw material selection, a catalytic system and process conditions, the method remarkably shortens the synthesis route, simplifies the operation process, effectively avoids potential safety hazards and environmental protection problems of a traditional process, and reduces the production cost. After the process is optimized, the raw material utilization rate is increased, the catalyst cost is reduced, the single-batch production cost is remarkably reduced, the product yield reaches 88% or above, the purity exceeds 99.5%, and the optical purity gt is obtained; therefore, the requirements of industrial production on high efficiency, economical efficiency and green sustainability are completely met.

The invention belongs to the technical field of synthesis and application of new compounds, and discloses a preparation method of 3, 3 '-diphenyl-1, 3, 4 According to the method, a quinoline derivative is adopted as a reaction substrate, an enamine intermediate is generated under the combined action of an activating reagent and a tert-butyl Grignard reagent under the acidic condition, then the enamine intermediate reacts with N, N-dimethyl chloro-ene imine to generate the 3, 3 '-biquinoline methane derivative, and the 3, 3'-biaryl heterocycle methane derivative is synthesized through the high-efficiency synthesis method of the 3, 3 '-biaryl heterocycle methane derivative and the high-efficiency synthesis method of the 3, 3'-biaryl heterocycle methane derivative. Or the enamine intermediate reacts with N, N-dimethyl chloroeneimine and an indole derivative to generate the 3, 3 '-bisheteroaromatic methane derivative. The method disclosed by the invention has the advantages of cheap and easily available reaction substrates, wide substrate range, greenness, neutral oxidation reduction, high atom economy and the like. According to the method disclosed by the invention, bisheteroaromatic methane substituted at different positions can be obtained, and the method is suitable for various substituent groups. The device can be popularized and used according to the principle, and the applicability is good.

The invention belongs to the technical field of organic compound synthesis, and particularly relates to a method for preparing an electron-deficient 1, 3-substituted benzene ring fluorine-containing compound through photo-cobalt concerted catalysis. Under the action of a composite catalyst, enamine and fluorine-containing aryl butadiene are promoted to react, and the composite catalyst is formed by mixing a visible light catalyst and a metal catalyst. The photocatalyst has the advantages that the reaction process is safe and controllable, and the preparation and production operation is simplified; a Kessil lamp is used as a reaction light source, is safe and environment-friendly, has high energy utilization efficiency, and can efficiently realize conversion from light energy to chemical energy; the used raw materials are low in price and easy to obtain, and the preparation process is simple. The process is mild in condition and good in regioselectivity, a series of electron-deficient group substituted [1, 3]-benzene ring fluorine-containing compounds can be efficiently obtained only through one-step reaction, and designability and application prospects of the compounds are greatly expanded.

The invention relates to the technical field of solid rocket propellants, and particularly discloses a neutral bonding agent containing an enamine structure and a preparation method and application of the neutral bonding agent. Glycidyl acrylate and cyanoethyl modified polyene polyamine epoxy ring-opening product, butyl acrylate and hydroxyethyl acrylate are adopted as polymeric monomers, and the neutral bonding agent containing the enamine structure and the preparation method and application of the neutral bonding agent containing the enamine structure are obtained. According to the prepared neutral bonding agent containing the enamine structure, amino in the molecular structure and ammonium perchlorate are easily subjected to acid-base neutralization to form ionic bonding, and a tear-resistant layer is formed; and meanwhile, the molecule also contains cyanoethyl which is far away from the main chain of the neutral bonding agent, so that the bonding effect on a nitramine oxidizing agent is relatively good. According to the invention, the problem that the mechanical property of the NEPE propellant formula is reduced due to introduction of ammonium perchlorate is solved.