115 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 an enamine pentafluorosulfhydrylation method using sulfur hexafluoride as a pentafluorosulfenyl source, which comprises the following steps: placing a photocatalyst and an alkaline additive in a reaction device, replacing air in the reaction device by using sulfur hexafluoride gas, adding enamine substances and a solvent in the atmosphere of the sulfur hexafluoride gas, and reacting at the temperature of 60-80 DEG C for 1-2 hours to obtain the enamine pentafluorosulfhydrylation product. Sealing the reaction device, carrying out photocatalytic reaction under a light source with the wavelength of 380-400nm, and then adding hydrochloric acid to obtain the pentafluorosulfenyl product. According to the method, the sulfur hexafluoride is used as a safe and cheap pentafluorosulfenyl reagent and acts with specific enamine substances to prepare the high-added-value organic pentafluorosulfenyl group-containing small molecules, the sulfur hexafluoride is ingeniously used as a fluorination reagent in the method, so that the pentafluorosulfenyl reaction is safely, economically and mildly carried out, and the yield of the pentafluorosulfenyl group-containing small molecules is improved. Meanwhile, wide substrate compatibility is shown, so that a green and efficient new way is provided for chemical synthesis in the field.

The invention relates to the field of medicine synthesis and preparation, in particular to a synthesis method of toxyanib phosphate. The use amount of acetic acid is greatly reduced in the preparation process, so that excessive acid does not need to be neutralized in the post-treatment process, and a large amount of wastewater is not generated; in addition, the use amount of sodium nitrite is reduced, and the environment and health are facilitated; the enamine reduction reaction does not use acetic acid as a solvent and a hydrogenation reaction catalyzed by heavy metal palladium, so that the safety of the reaction is improved, and the purity of the product is also improved; a decarboxylation reaction and a Vilsmeier-Haack reaction are carried out by a one-pot method, so that the reaction steps are reduced, and the product purity is improved; when aldol reaction is carried out in side chain splicing, side reaction and generation of isomer impurities are reduced. The method is short in route, mild in reaction condition, low in equipment requirement and convenient to operate, industrial production is easy to achieve, and a complex purification method is not needed.

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 discloses a dynamic polyene amine compound as well as a preparation method and application thereof. The structural formula of the dynamic polyene amine compound is as shown in formula (I). The dynamic polyenamine compound is obtained by carrying out polymerization reaction on a binary amide activated alkynyl compound and a diamine compound in an organic solvent. The preparation method has the advantages of mild reaction conditions, no need of catalyst, simple and easily available raw materials, high atom utilization rate, high polymer yield, high molecular weight and excellent stereoselectivity. The dynamic polyene amine compound prepared by the invention has the properties of good processability, film-forming property, high thermal stability, non-traditional luminescence and the like, and the dynamic enamine bond contained in the dynamic polyene amine compound prepared by the invention can realize accurate degradation and structural replacement of a polymer under mild conditions.

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 superstrong solid base catalyst as well as a preparation method and application thereof. Mesoporous nano MgO is obtained through urea-assisted precipitation and air atmosphere calcination, then the freshly prepared mesoporous nano MgO is soaked in an alkali metal salt solution, and a series of superstrong solid base catalysts with different alkali metal loading capacities are obtained through calcination and activation. Beta-carbon glycoside ketone and an aldehyde compound raw material without alpha hydrogen are subjected to aldol condensation reaction under the promotion of the prepared superstrong solid base catalyst to obtain a carbon glycoside product with an alpha, beta-unsaturated carbonyl structure, the separation yield of the product is 90% or above, and the reaction performance is not obviously reduced after the catalyst is recycled for ten times. The method has the advantages that the method is simple in operation and low in cost, has super-strong alkaline sites, can efficiently catalyze the aldol condensation reaction of the beta-carbon glycoside ketone to obtain the target product carbon glycoside without the assistance of amine compounds to form enamine, and is simple in reaction system separation, reusable, green in process, simple to operate and suitable for industrial production.

The invention discloses a triptycene modified beta-ketoenamine covalent organic framework as well as a preparation method and application thereof, and the triptycene modified beta-ketoenamine covalent organic framework is prepared by polycondensation of a polyamino triptycene monomer, a 1, 3, 5-trialdehyde phloroglucinol monomer and an enamine monomer. The triptycene modified beta-ketoenamine covalent organic framework disclosed by the invention has excellent performance of photocatalytic decomposition of water to produce hydrogen, and can be repeatedly used. The preparation method provided by the invention is simple in process, mild in condition, short in time consumption, environment-friendly and easy for industrial production.

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 relates to the field of hygienic products, provides a bacteriostatic absorption core body and a preparation method thereof, and solves the problems that an existing bacteriostatic absorption core body does not have an anticoagulation function, and Ag < + > is easy to migrate to a human body in a manner of coating and adding Ag < + > or the bacteriostatic effect is relatively poor in a manner of coating and adding Ag < + >. The antibacterial absorption core body comprises a lower non-woven fabric layer, an SAP and modified PET fiber mixture layer, a sizing layer and an upper non-woven fabric layer which are sequentially laminated from bottom to top; wherein the SAP and modified PET fiber mixture layer is obtained by mixing SAP and modified PET fibers and then carrying out negative pressure adsorption, conveying and forming, and the modified PET fibers comprise the following raw materials: acetone, absolute ethyl alcohol, PET fibers, sodium periodate, dopamine hydrochloride, N, N-dimethylformamide, propylene glycol monomethyl ether, a silver ammonia solution, azodiol enamine, hydrochloric acid, N, N-dimethylformamide and deionized water.

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 present invention discloses the preparation method of β-phosphonyl-enamine derivative. The preparation method comprising the following steps: dissolving the enamine derivative, organic phosphine compound, manganese acetate and potassium carbonate in the solvent, reacting at room temperature to obtain the β-phosphonyl-enamine derivative. The enamine derivative was as the starting material, and the raw materials are easy to obtain and a great many varieties. The various forms of the products obtained therein can be directly applied and can be used in further reactions. The reaction conditions are mild, the reaction speed is high, the reaction operation and the post-treatment process are simple, the production is convenient, and the method is suitable for large-scale production.

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.

The invention belongs to the technical field of electrocatalysis, and particularly relates to application of a carbon cloth loaded nonmetal COF material EN-COF electrode in electrochemical synthesis of urea. The porous organic material EN-COF catalyst is synthesized by taking an enaminone structure as a connecting unit and taking TDOEB and TAPT as raw materials. The catalyst is prepared into printing ink, carbon cloth is smeared with the printing ink, a carbon cloth loaded nonmetal COF material EN-COF electrode is prepared, the electrode is used for electrocatalytic urea production, the Faraday efficiency is 38.69% under-0.5 V vs.RHE, continuous electrolysis is conducted for 11 h, and the current density is stabilized at 0.6 mA cm <-2 >. The material has relatively high Faraday efficiency under the conditions that no metal participates and CO2 and NO3 <-> solutions are respectively used as a carbon source and a nitrogen source, shows relatively good electrocatalytic activity and stability, and has a wide application prospect in the field of electrochemical C-N coupling synthesis of urea.

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.

The invention provides a process for synthesizing enamine from 2-methyl-4-amino-5-formylaminomethylpyrimidine mother liquor and application of the process, and relates to the technical field of enamine condensation. Comprising the following steps: carrying out enamine condensation reaction on the 2-methyl-4-amino-5-formylaminomethylpyrimidine mother liquor and alpha-sodium formyl-beta-formylaminopropionitrile under an acidic condition, so as to obtain enamine; the 2-methyl-4-amino-5-formylaminomethylpyrimidine mother liquor is a mother liquor obtained by a reaction of alpha-(o-chloroaniline)-based methine-beta-formylaminopropionitrile and an acetamidine solution. The method solves the technical problems that in the prior art, the energy consumption for recovering o-chloroaniline from the 2-methyl-4-amino-5-formylaminomethylpyrimidine mother liquor is large, the recovery is not thorough, and enamine contained in the mother liquor cannot be recycled, and achieves the purposes of reducing the recovery energy consumption, thoroughly recovering o-chloroaniline, improving the recovery efficiency and the like. The enamine contained in the mother liquor is subjected to resource utilization; and the product yield is improved.