90 results about "Enamine" patented technology

The invention belongs to the technical field of pyrimidine [1, 2-b] indazole derivative synthesis, and particularly relates to a fluoro pyrimidine [1, 2-b] indazole compound and a preparation method thereof. The preparation method specifically comprises the following steps: by taking an enamine compound as shown in a formula 1, heteroarylamine as shown in a formula 2 and polyfluoroalkyl halide as shown in a formula 3 as reaction substrates, mixing the reaction substrates, a catalyst and a solvent, and carrying out cyclization reaction in a protective gas atmosphere and under blue light irradiation to obtain the fluoropyrimidine [1, 2-b] indazole compound. The fluorine atom substituted or multi-fluoroalkyl substituted pyrimidine [1, 2-b] indazole derivative can be selectively constructed in the same reaction system, the diversity of the structure is obviously expanded, and the reaction conditions are mild and green and environment-friendly.

The invention discloses a vinylidene bridged covalent organic framework material based on 2, 7-diaza pyrene and a preparation method thereof.The 2, 7-diaza pyrene is used as a core monomer, under the catalysis of benzoic acid and benzoic anhydride, methyl is activated to form an enamine intermediate, aryl aldehyde is attacked to form unsubstituted carbon-carbon double bonds, and under the heating condition, the 2, 7-diaza pyrene is synthesized into the vinylidene bridged covalent organic framework material based on 2, 7-diaza pyrene. And two vinylidene bridged COFs materials with high crystallinity are successfully synthesized. The COFs material disclosed by the invention has a high specific surface area, a uniform through rhombic pore channel structure and excellent chemical stability, and has an important application prospect in the field of photoelectrocatalysis.

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 provides a ketone-enol tautomeric structure catalyst as well as a preparation method and application thereof in photosynthesis of hydrogen peroxide, and belongs to the technical field of catalysts. The preparation method comprises the following steps: mixing a first organic linker, a second organic linker, an acid catalyst and an organic solvent, and carrying out solvothermal reaction to obtain the ketone-enol tautomeric structure catalyst. According to the beta-keto-enamine COFs and the preparation method thereof, keto-enol tautomerism can be effectively adjusted through integration of different amounts of-OH groups in the beta-keto-enamine COFs, so that the visible light absorption capacity and the charge generation efficiency of the COFs are improved. When the keto-enol tautomeric structure catalyst provided by the invention is used for photosynthesis of hydrogen peroxide, water and oxygen can be effectively activated, so that the keto-enol tautomeric structure catalyst shows excellent hydrogen peroxide photosynthesis activity. The result of the embodiment shows that the H2O2 production rate of the ketone-enol tautomeric structure catalyst provided by the invention can reach 3474 mu mol / gcat <-1 > h <-1 >.

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 invention provides a waterborne epoxy curing agent based on enamine bonds as well as a preparation method and application of the waterborne epoxy curing agent, and belongs to the technical field of coatings. The waterborne epoxy curing agent based on the enamine bond is prepared from the following raw materials in parts by weight: 12 to 14 parts of a polyepoxy compound, 7 to 12 parts of a polyamine compound, 37 to 42 parts of a polyether-based polyacetoacetate compound, 9 to 14 parts of a diacetoacetate compound, 5 to 7 parts of a monoacetoacetate compound and 20 to 50 parts of a solvent. According to the waterborne epoxy curing agent constructed through enamine bonds, the free amine content of the obtained waterborne epoxy curing agent can be effectively reduced, and the activation period of the waterborne epoxy curing agent during use is prolonged.

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.

According to the method, an enamine intermediate (2Z)-4-oxo-4-[3-(trifluoromethyl)-5, 6-dihydro-[1, 2, 4] triazolo [4, 3-a] pyrazine-7 (8H)-yl]-1-(2, 4, 5-trifluorophenyl) butyl-2-ene-2-amine is used as an initial raw material, and the Sitagliptin is synthesized through synergistic catalysis asymmetric hydrogenation of a cobalt catalyst and a chiral ligand. The R-configuration sitagliptin is prepared by one step, the reaction yield and stereoselectivity are high, the catalytic reaction effect is good, the cost is low, and the method is suitable for industrial large-scale production.

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.

The invention discloses a preparation method of a thiapyran-4-ketone compound, which comprises the following steps: taking an enaminone compound with a chemical structural formula as shown in a formula (I) and a sulfur source compound as raw materials, reacting for 12-24 hours in a solvent at 90-120 DEG C under the action of a catalyst to obtain a reaction product, and then purifying the reaction product to obtain the thiapyran-4-ketone compound. The structural formula of the thiapyran-4-ketone compound is shown as a formula (II). The preparation method disclosed by the invention has the characteristics of low raw material cost, mild reaction conditions, simplicity in operation, few reaction byproducts, environment friendliness and the like, thereby having a wide application prospect.

The invention relates to the technical field of lubricating oil, and discloses galvanized metal forming lubricating oil and a preparation method thereof.The lubricating oil is prepared from, by mass, 10%-15% of a modified graphene lubricating agent, 8%-12% of an oiliness agent, 5%-10% of an anti-rust agent, 0.1%-0.5% of a corrosion inhibition additive, 0.1%-0.3% of an antioxidant and the balance base oil and inevitable impurities; the modified graphene lubricant is obtained by modifying graphene oxide with enamine; the preparation method comprises the following steps: adding the modified graphene lubricant, the oiliness agent, the antirust agent, the corrosion inhibition additive, the antioxidant and the base oil into a container, and uniformly stirring at 55-60 DEG C to obtain the galvanized metal forming lubricating oil. The modified graphene is obtained through enamine modified graphene oxide, the indissolvable property of graphene in an organic solvent can be improved, and the modified graphene is added into the galvanized metal forming lubricating oil, so that the stability of the lubricating oil is improved.

The present invention provides a catalyst for the regeneration of a dehydrating agent for 2-cyanopyridine and a preparation method thereof, belonging to the technical field of catalysts; the catalyst comprises, by weight percentage: 0.5-10% of a metal oxide, 0.5-3% of MgO-SiO2, and the balance being a carrier; the metal oxide contains In and Sn; the weight percentage of MgO in MgO-SiO2 is 30%-75%; in the catalyst of the present invention, through two impregnations, the carbonyl group in the amide is activated by two metal ions, In and Sn, and the magnesium oxide acting through SiO2 effectively activates hydrogen atoms and stabilizes the enamine intermediate, so that the reaction can dehydrate efficiently to obtain the target product; when the catalyst of the present invention is used in the regeneration reaction of the dehydrating agent for 2-cyanopyridine, the conversion rate of 2-pyridinecarboxamide can reach 80-98%, and the selectivity of 2-cyanopyridine > 99%, which is significantly higher than that of the same type of dehydrating catalyst.

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.

The invention discloses a preparation method of 9,10-phenanthrenequinone compounds, comprising the following steps: using an enaminone compound as shown in a chemical structure formula (I) as a raw material, under a protective gas environment, in the presence of a small molecule catalyst and an oxidant, reacting for 2 to 12 hours at 30 to 90 ° C in an organic solvent to obtain a reaction product, and then purifying the resulting reaction product to obtain a chemical structure formula (II) as shown in 9,10-phenanthrenequinone compounds. The present invention uses an enaminone compound as a raw material, which is a raw material with simple synthesis and high conversion rate, a wide range of substrate applications, low raw material and catalyst costs, low pollution, few reaction byproducts, and has the characteristics of green environmental protection; in addition, the reaction conditions required for the inventive method are very mild, the number of reactions is small, the operation is simple, and the yield is high.

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

The present invention relates to a method for synthesizing sitagliptin through cobalt-catalyzed asymmetric hydrogenation. The method uses an enamine intermediate (2Z)-4-oxo-4-[3-(trifluoromethyl)-5,6-dihydro-[1,2,4]triazolo[4,3-a]pyrazine-7(8H)-yl]-1-(2,4,5-trifluorophenyl)but-2-en-2-amine as a starting material, and carries out asymmetric hydrogenation through the coordinated catalysis of a cobalt catalyst and a chiral ligand to prepare R-configured sitagliptin in one step. The method has high reaction yield and stereoselectivity, good catalytic reaction effect, low cost, and is suitable for industrial scale-up production.

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.

The invention belongs to the technical field of adsorption materials, and relates to a carboxyl / amidoxime functionalized ribbon-shaped beta-keto-enamine covalent organic framework material, a preparation method and application thereof, the preparation method comprises the following steps: (a) in a catalyst and solvent system, enabling trialdehyde phloroglucinol to react with 2, 5-diaminobenzonitrile and 2, 5-diaminobenzonitrile containing carboxylic acid, sulfonic acid or phosphate groups to obtain a covalent organic framework material; the preparation method comprises the following steps: carrying out condensation reaction on 2, 5-diaminobenzene derivatives to form a ribbon-shaped covalent organic framework material containing carboxyl and nitrile groups; and (b) carrying out oximation reaction, and converting the cyano group into an amidoxime group to obtain the carboxyl / amidoxime functionalized ribbon-shaped beta-keto-enamine covalent organic framework material. According to the carboxyl / amidoxime functionalized ribbon-shaped beta-ketoenamine covalent organic framework material disclosed by the invention, the adsorption capacity of the material is improved, the selectivity to uranyl ions is improved, the material is an adsorbent material with excellent adsorption performance to uranium, and the practical application of the covalent organic framework material in the field of extraction of uranium from seawater is promoted.

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.