843 results about "Atom economy" patented technology

The invention discloses a foam iron-nickel surface in-situ growth platinum modified nickel-iron layered double hydroxide bifunctional material and a preparation method and application thereof.The preparation method comprises the steps that a foam iron-nickel substrate is immersed in an acid solution containing chloroplatinic acid, heating treatment is conducted for a certain period of time, and then the nickel-iron layered double hydroxide bifunctional material is obtained; and a nickel-iron layered double-metal hydroxide mixed material modified by platinum nanoparticles grows on the surface of the foam iron-nickel in situ. In the preparation process of the one-step method, nickel ions or / and iron ion salts and sacrificial agents do not need to be additionally added, atom economy is good, reaction conditions are mild, energy consumption is low, and meanwhile the problem that the catalyst is prone to falling off due to multiple times of operation and washing is solved. The platinum / ferronickel layered bimetal hydroxide / foam iron nickel electrode prepared by the method shows excellent hydrogen production and oxygen production activity in an alkaline water electrolysis reaction.

The present invention provides a preparation method of 4,6-dihydroxypyrimidine, and the preparation method comprises the following steps: adding a mixed solution of malonate and formamide to an alkali metal alcoholate / solvent containing a catalyst, and then keeping the mixture warm for reaction after the addition is completed. After the reaction is completed, the solvent is evaporated to dryness, and after being dissolved in water, the mixture is acidified to a pH of 2-3, filtered, washed with water, and dried to obtain 4,6-dihydroxypyrimidine. The present invention utilizes a catalyst to catalyze the reaction, thereby improving the reaction yield, having a high atomic economy, and reducing the amount of raw materials used, reducing the generation of saline wastewater, and alleviating environmental pressure.

The invention relates to the field of medicine synthesis, and particularly discloses a preparation method of abesilib and an intermediate thereof. The invention relates to an abesiril intermediate, which is 4-chloro-5-fluoro-2-(methylsulfonyl) pyrimidine (IV) and 4-fluoro-6-(5-fluoro-2-(methylsulfonyl) pyrimidine-4-yl)-1-isopropyl-2-methyl-1H-benzo [d] imidazole (V). The invention further provides a preparation method of the abesiril intermediate. And carrying out nucleophilic substitution reaction on the abesilib intermediate V and 5-[(4-ethyl piperazine-1-yl) methyl] pyridine-2-amine to prepare the abesilib. According to the preparation method, the raw materials are cheap and easy to obtain, the reaction selectivity of functional groups is high, ectopic impurities generated by a halogen atom competition reaction are effectively avoided, meanwhile, introduction of heavy metal palladium can be reduced, and therefore the cost is reduced. The synthetic route is simple, the atom economy is high, the controllability in production is high, and the method is suitable for industrial production.

The invention relates to the field of organic photoelectricity, and discloses an asymmetric benzotriazole high-efficiency fluorescent isomer for a light conversion film and a synthesis method of the asymmetric benzotriazole high-efficiency fluorescent isomer. The optimal excitation wavelength of the compound is about 280-290 nm, the maximum absorption peak is about 280-350 nm, the strongest emission peak is about 370-440 nm, and the molar extinction coefficient is greater than 20000 L / (mol.cm). The proportion of two isomers generated during hydrogen substitution on a nitrogen atom of benzotriazole is close to 1: 1, and at present, only symmetric products are utilized in most researches, so that the research blank of asymmetric isomers is filled, and the asymmetric products are proved to have efficient fluorescence performance. When the light conversion film is prepared, the asymmetric product can be independently used as a light conversion agent, and the two isomers can be blended according to any proportion to be used as the light conversion agent, so that the atom economy is fully improved, and the method has great significance on future basic research and industrial application.

The invention develops an efficient conversion method for synthesizing the anti-schizophrenia drug blonanserin. According to the preparation method, commercially available cyclooctanone, 1-(4-fluorophenyl) prop-2-ene-1-ketone and NH4X (X = F, Cl, Br or I) are subjected to a three-component [2 + 1 + 3] form cascade cyclization method, then m-CPBA is used for oxidation to obtain nitrogen oxide, and finally the nitrogen oxide reacts with N-ethyl piperazine to obtain the blonanserin compound. The two methods respectively obtain the functional group tolerant blonanserin compound with high yield. The two interesting methods have the characteristics of simple operation, easily available starting materials, mild reaction conditions, good functional group tolerance, high atom economy and the like. In addition, compared with a traditional method (at least five steps are needed), the strategy can provide a good synthesis route for the anti-schizophrenia drug blonanserin with a highly functionalized structure.

The present invention relates to the field of medical technology, and in particular to a semaglutide intermediate and a preparation method thereof, and a method for synthesizing semaglutide. The present invention screens different solvent combinations, finds a reaction system compatible with side chain tetrapeptide modification, main chain dipeptide modification and deprotection steps, and synthesizes semaglutide using a "one-pot method". The method does not require separation of any intermediate, does not involve complex operations such as isoelectric elution, separation, and redissolution of the intermediate, is simple to operate, has a high yield, and is conducive to industrial scale-up production. Further, the present invention uses a double Fmoc-protected dipeptide: Fmoc-His(Fmoc)-Aib-OH replaces Fmoc-His-Aib-OH·TFA as a starting material, which greatly reduces the use of Fmoc-His(Fmoc)-Aib-OH, and the feed amount is reduced from 8 to 10 times to 1 to 3 times, the atomic economy is increased, and the production cost is reduced.

The invention provides a preparation method of rotaxane mechanical interlocking molecules. According to the preparation method, under the condition of not adding a catalyst, dibenzene-24-crown-8, benzene-21-crown-7, an isocyanate derivative and a rod-shaped compound are subjected to a reaction by adopting a one-pot method to obtain the rotaxane mechanical interlocking molecule. The preparation method not only can reach 100% of atom economy and meet the requirements of green chemistry, but also can reach the yield of 65% or above, and realizes efficient preparation of rotaxane mechanical interlocking molecules.

The invention belongs to the field of biological catalysis, and particularly relates to a method for preparing oxidized nicotinamide adenine dinucleotide phosphate through double-enzyme coupling. According to the invention, through construction and optimization of a one-pot double-enzyme coupled catalytic system, a genetically engineered bacterium containing nicotinamide mononucleotide adenosine transferase NMNAT and a genetically engineered bacterium containing NAD kinase are used as a whole-cell catalyst, nicotinamide mononucleotide NMN is used as a starting substrate, adenosine triphosphate, polyphosphate and divalent metal ion salt are added, and the whole-cell enzyme is prepared through a one-pot method. The oxidized nicotinamide adenine dinucleotide phosphate NADP < + > is efficiently and catalytically synthesized by a one-pot method, and the whole-cell catalytic reaction liquid is separated and purified to obtain the NADP < + >. The double-enzyme catalysis method disclosed by the invention is short in reaction route, high in atom economy, capable of reducing the existing production cost, short in production period, easy for downstream separation and purification, and suitable for large-scale and large-scale production of NADP < + >.

The invention discloses a synthesis method of a 6-trifluoromethylthio phenanthridine compound, and belongs to the technical field of organic synthesis. The phenanthridine compound containing the trifluoromethylthio group is prepared in one step by taking phenanthridine thione as a raw material and taking bromotrifluoromethane which is low in price and easy to obtain as a fluorinating reagent through a C = S free radical addition reaction under the action of visible light induction and a photocatalyst and alkali. The method has the characteristics of being green and safe, cheap and easily available in raw materials, high in atom economy, good in reaction regioselectivity, mild in reaction condition, wide in substrate application range, high in yield, easy in product purification and the like, and belongs to green synthesis.

The invention discloses a synthesis method of an unsaturated ketone or arone compound, which comprises the following steps: at a certain temperature, taking unsaturated hydrocarbon or aromatic hydrocarbon as a raw material, taking an N-hydroxyimide compound as a catalyst, adding an organic solvent for dissolving, introducing oxygen or air into a reaction solution under the irradiation of visible light, and carrying out oxidation reaction to obtain the unsaturated ketone or arone compound. And carrying out post-treatment separation to obtain the unsaturated ketone or arone. According to the method, air, oxygen-enriched gas or oxygen is used as a harmless oxidizing agent, visible light is used as an energy source to promote the reaction, and the method has the advantages that the reaction process is green and efficient, the cost is low, the dosage of the catalyst is small, and most of the catalyst can be recycled and reused; the atom economy is high.

The invention provides a deuterium-labeled 3-indoleacrylic acid isotope compound and a preparation method thereof, and relates to the technical field of plant hormone detection, deuterated toluene is creatively nitrated and subjected to a ring closing reaction, then an aldehyde group is introduced, and finally hydrolysis is performed to obtain the target product deuterium-labeled 3-indoleacrylic acid isotope compound. The preparation method provided by the invention is strong in operability, relatively good in atom economy and excellent in reproducibility and stability, the isotope abundance of the prepared deuterium-labeled 3-indoleacrylic acid isotope compound can reach 98% or above, the chemical purity is 98% or above, and the deuterium-labeled 3-indoleacrylic acid isotope compound can be used as an internal standard substance for detecting plant hormones and has good application prospects. The method has important practical application value.

The invention belongs to the technical field of organic synthesis and carbene catalysts, and particularly relates to a bridged double-center carbene catalyst ligand as well as a preparation method and application thereof. The structure of the bridged double-center carbene catalyst ligand is as shown in a formula I: # imgabs0 #, in the formula I, R1, R3, R4, R5, R6, R7, R8, R9 and R10 are respectively and independently selected from any one of H, i-Pr, CH3, Cl, F and NC; n is equal to 1-9; n is selected from any one of Cl and Br. Compared with a carbene catalyst ligand used in the past, the bridged double-center carbene catalyst ligand provided by the invention has double active centers, so that the double-center carbene catalyst ligand can be used for preparing the double-active-center carbene catalyst ligand, and the double-active-center carbene catalyst ligand can be used for preparing the double-active-center carbene catalyst ligand; and by carrying out ligand exchange with a carbene catalyst precursor with a single active center, the active center can be aggregated, so that the high-activity carbene catalyst with double centers is obtained, and higher reaction activity and atom economy are achieved.

The invention relates to an aliphatic copolyester elastomer and a preparation method thereof, and belongs to the field of high polymer materials. The elastomer is prepared through a series ring-opening copolymerization reaction of epoxide and cyclic anhydride, and the method comprises the following steps: under the action of a metal-free catalyst (a phosphazene ligand P1-tert-octyl / triethyl boron system) and an initiator (terephthalyl alcohol), carrying out a series ring-opening copolymerization reaction on epoxide and cyclic anhydride, the preparation method comprises the following steps: reacting epoxide (such as epoxypropane and allyl glycidyl ether) with aliphatic anhydride (such as glutaric anhydride) in a xylene solvent to generate a polyester prepolymer retaining an active end; adding a second group of epoxide (such as cyclohexene oxide) and anhydride (such as tetrahydrophthalic anhydride and norbornene dianhydride), continuously reacting to form a block copolymer, and then crosslinking. The material performance can be regulated by changing the monomer combination, the atom economy is high, and the raw materials can be produced on a large scale. The process is simple and environment-friendly, and a new choice is provided for application of the degradable elastomer in the fields of medical treatment, environmental protection and the like.

Disclosed in the present invention are a hard carbon material and a preparation method therefor and the use thereof, and a battery. The preparation method for the hard carbon material comprises: mixing a solution containing PVC and an aromatic compound under heating conditions until a solvent is completely evaporated to dryness, so as to obtain an xerogel, wherein the mass ratio of the aromatic compound to the PVC is 2-25%; grinding, washing and drying the xerogel, so as to obtain a dehalogenated-PVC precursor; and carbonizing the dehalogenated-PVC precursor, so as to obtain the hard carbon material, wherein the carbonization is performed at a temperature of 700-1200°C for 1-4 h. The hard carbon material prepared in the present invention has relatively high atom economy and high electron conductivity, and has good electrochemical performance when being used for the preparation of a battery.

The present invention discloses a method for synthesizing rasagiline in a microfluidic field. The method is based on a double enzyme hydrogenation cascade reaction, which efficiently converts racemic alcohol into enantiomeric amines, realizes the direct synthesis of chiral amines, and has high atom economy and reaction efficiency. Racemic 1-indanol is completely oxidized to generate 1-indanone by alcohol dehydrogenase catalysis, and the cofactor NADP+ is reduced to NADPH to provide the required reducing power for subsequent reactions; using ( R )-selective reductive amino enzyme catalyzes the reductive amination reaction of 1-indanone to generate the target product rasagiline. The present invention adopts a dual enzyme synergistic catalytic strategy to successfully achieve the efficient conversion from racemic alcohol to chiral amine, has the advantages of mild reaction conditions, green sustainability, high product yield and optical purity, and provides a new efficient, economical and environmentally friendly way for the synthesis of rasagiline.

The application discloses a catalyst for preparing polyoxymethylene dimethyl ethers by directly oxidizing methanol, a preparation method and application thereof, and belongs to the field of catalyst preparation and application. The metal oxide and the acidic molecular sieve are effectively coupled to prepare a bifunctional composite catalyst with a core-shell structure, the composition and proportion of the metal oxide and the acidic molecular sieve are regulated, and high-selectivity synthesis of polyoxymethylene dimethyl ethers by directly oxidizing methanol is realized. The unique core-shell structure can effectively regulate the distance and distribution between the two types of active sites, significantly promote the gradual chain growth of methanol oxidation, and obviously inhibit the occurrence of side reactions such as methanol dehydration to dimethyl ether and deep methanol oxidation, so that the high-selectivity synthesis of polyoxymethylene dimethyl ethers by directly oxidizing methanol is realized. The catalyst preparation process is simple and easy to operate, and the one-step oxidation of methanol to prepare polyoxymethylene dimethyl ethers has the advantages of short flow, good atom economy and green process.

The invention belongs to the technical field of organic synthesis, and relates to a preparation method of 5, 5-dimethyl-4, 5-dihydroisoxazole. The method comprises the following steps: (1) reacting isopentenal with an oximation agent to obtain a reaction solution containing isopentenal oxime; (2) dropwise adding the reaction liquid into a mixture containing isopentenal and an acid catalyst for reaction to obtain a product; or when the reaction liquid contains water, performing phase splitting on the reaction liquid to obtain an organic phase, and dropwise adding the organic phase into a mixture containing the isopentenal and the acid catalyst for reaction to obtain a product. The method does not produce ketone by-products, and is good in atom economy, high in reaction yield, good in technological process continuity, low in cost, few in materials, simple to operate, mild in reaction condition, low in requirements on production equipment and suitable for large-scale industrial production.

The invention discloses a preparation method of meta-phosphorylated polysubstituted pyridine compounds, and belongs to the technical field of organic synthesis. The synthesis process is simple, highly toxic reagents, various catalysts and expensive noble metal catalysts do not need to be used, tert-olefin amide and an organophosphorus reagent are used as basic raw materials, manganese acetate is used as an accelerant (conventional reaction reagents, solvents and accelerants are utilized), and the tert-olefin amide is synthesized through an intramolecular free radical cascade reaction. The meta-phosphorylated polysubstituted pyridine compound can be efficiently obtained in one step, and the yield is as high as 95%; in addition, the reaction raw materials are cheap and easy to obtain, the atom economy is high, the substrate universality is wide, and the operability is high. The meta-phosphorylated polysubstituted pyridine compound disclosed by the invention has relatively good insecticidal activity on beet armyworm larvae, and can be applied to agricultural pest control as an insecticide.

The present invention belongs to the technical field of organic synthesis, and provides an electrochemical synthesis method for N-aroyl amide compounds, which comprises the following steps: (1) in an electrochemical reaction device containing an aromatic hydrocarbon compound, an electrolyte and a nitrile solvent, a pre-oxidant is added, and then the anode and the cathode are assembled for electrolysis reaction; (2) after the reaction is completed, a saturated NaHCO3 solution is slowly added dropwise directly into the electrochemical reaction device for hydrolysis reaction to obtain the required N-aroyl amide compounds, wherein the pre-oxidant is selected from any one or more of acids, sulfates or persulfates. The electrochemical synthesis method of the present invention does not require the introduction of a directing group or pre-functionalization of the substrate, avoids the use of metal catalysts and the application of stoichiometric oxidants, has the advantages of greenness, high efficiency, high atom economy, etc., can be used for the synthesis of drug acetanilide, and has certain practical application value.

The invention discloses a method for preparing a biological hydrocarbon compound by organic photocatalysis higher fatty acid decarboxylation, which comprises the following steps: adding higher fatty acid, a hydrogen atom transfer catalyst and an acridine photocatalyst / solid-phase acridine photocatalyst into a reaction solvent, stirring and reacting for 12-24 hours under the conditions of blue light irradiation and room temperature to obtain a reaction solution, filtering, washing and drying to obtain the biological hydrocarbon compound. And removing the reaction solvent of the obtained reaction solution under reduced pressure, and purifying by thin layer chromatography / column chromatography to obtain the long-chain alkane compound after decarboxylation of the higher fatty acid. The method is simple in step, mild in reaction condition and high in product yield, does not use any metal compound, and has the characteristics of high atom economy and environmental protection. And for unsaturated carboxylic acid, olefin configuration before and after decarboxylation is not influenced. When solid-phase acridine is used as a photocatalyst for reaction, the catalyst can be recycled through simple washing, filtering and recycling, excellent catalytic activity can still be kept after the catalyst is recycled for more than 10 times, and the reaction cost is further reduced.

Improved processes are provided for efficient production of elacestrant and intermediates thereof, enabling higher atom economy, improved safety, reduced consumption of palladium catalysts, and easier purification.

The invention discloses a large-steric-hindrance nitrile compound and a preparation method and application thereof.The preparation method comprises the steps that indole carbonate and benzyl isocyanide serve as reaction raw materials, and the nitrile compound with a large-steric-hindrance quaternary carbon center is prepared through a one-pot method in the presence of a metal salt catalyst and a solvent; the invention provides a large-steric-hindrance nitrile compound which has the advantages of higher step economy, atom economy, convenience in post-treatment, rapidness and high efficiency. The high-steric-hindrance nitrile compound is constructed in one step by using simple raw materials, has the advantages of cheap and easily available raw materials, simple and mild conditions, high atom economy, excellent yield and wide substrate range, provides a green synthesis method for efficient construction of a high-steric-hindrance nitrile compound skeleton, and is convenient for preparation of the high-steric-hindrance nitrile compound and application of the high-steric-hindrance nitrile compound in the field of drug preparation.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of 1, 3-divinyl-1, 1, 3, 3-tetramethyldisiloxane. The preparation method comprises the following steps: S1, acetylene and dimethylchlorosilane are subjected to a hydrosilylation reaction under the action of a platinum monatomic catalyst, and a mixture is obtained; s2, pressurizing the mixture to 0.1-0.2 MPa, and condensing through a condenser; s3, the gas phase is recycled, and the liquid phase part is subjected to rectification separation to obtain vinyl dimethyl chlorosilane; s4, carrying out countercurrent reaction on the vinyl dimethyl chlorosilane and water, so as to generate a 1, 3-divinyl-1, 1, 3, 3-tetramethyldisiloxane crude product and hydrochloric acid; and S5, rectifying the crude product to obtain a pure product. The invention provides the preparation method of the 1, 3-divinyl-1, 1, 3, 3-tetramethyldisiloxane, which is high in atom economy and simple and convenient to operate, and meanwhile, the requirements of high selectivity, low environmental load and low cost are met.

The invention belongs to the technical field of pesticide chemistry, and particularly relates to a preparation method of a penconazole active compound, which comprises the following steps: by taking 2-(2, 4-dichlorophenyl) valeraldehyde and 1, 2, 4-triazole as starting raw materials, condensing and reducing under the action of a catalyst to obtain a penconazole crude product, and recrystallizing to obtain the penconazole active compound. Compared with the prior art, the penconazole active compound prepared by the invention has the advantages that the conversion rate of the raw materials is greatly improved, the problem that a derivative is generated by using potassium borohydride as a reducing agent is solved, so that the penconazole has atom economy and environmental protection property, the process flow is simpler, the operation steps of subsequent treatment and the use of a solvent are reduced, and the cost is reduced. The method is simple in operation and low in energy consumption, impurities in the penconazole preparation process are effectively removed, the purification rate and the yield of the penconazole technical are greatly improved, and the strict requirements for high-quality pesticides in agricultural production are met.

The invention belongs to the technical field of organic synthesis, and discloses a synthesis method of polysubstituted 1, 3-conjugated diene. The synthesis method of the polysubstituted 1, 3-conjugated diene comprises the following steps: in a protective atmosphere, with an organic solvent as a reaction medium, carrying out a reaction on a carboxylic acid compound, isonitrile and propargyl ester under the action of a weakly alkaline salt, a catalyst and a ligand to obtain the polysubstituted 1, 3-conjugated diene. The structure of the polysubstituted 1, 3-conjugated diene is shown in the specification. The method is simple, the raw materials are cheap and easy to obtain, the polysubstituted 1, 3-conjugated diene compound with rich and diversified structures can be constructed in one step, the yield is high, the substrate applicability is wide, and the atom economy is high. # imgabs0 #

The invention discloses chiral boryl alcohol and a preparation method thereof, and belongs to the technical field of organic synthesis. The preparation method comprises the following step: in the presence of a catalyst and a transfer hydrogenation reagent, carrying out selective transfer hydrogenation reaction on acyl boron to generate chiral boryl alcohol. According to the method disclosed by the invention, the core skeleton of the chiral boryl alcohol is prepared with high selectivity through asymmetric transfer hydrogenation of acyl boron, the synthetic route is direct, and the atom economy is high; raw materials and catalysts are cheap and easy to obtain, reaction conditions are mild, operation is simple, and reaction is efficient.

The present invention belongs to the field of functional resins and specifically relates to a lignin-modified dicyclopentadiene phenol resin and a preparation method thereof. The present invention utilizes phenol to phenolate bamboo lignin under alkaline conditions, and then uses methanesulfonic acid to catalyze the reaction of the phenolated bamboo lignin, phenol, and dicyclopentadiene to prepare the dicyclopentadiene phenol resin. This reduces the amount of phenol used in the dicyclopentadiene phenol resin and improves its heat resistance, corrosion resistance, and other properties, resulting in high bonding strength, friction resistance, and electrical insulation. Furthermore, the preparation method is simple, the reaction conditions are mild, and the production cost is low, meeting the environmental protection needs of modern society while also adhering to the principles of green chemistry and chemical atom economy.

The invention discloses a preparation method of 6-nitro-m-cresol, and belongs to the technical field of organic synthesis.The method comprises the steps that raw materials are subjected to esterification, water washing, sulfonation, nitration, desulfonation and refining in sequence, and the 6-nitro-m-cresol is obtained. According to the method, it can be guaranteed that the intermediate product is the 6-nitro derivative, generation of isomer impurities such as 2-site and 4-site is greatly reduced from the source, the reaction path is clear, and atom economy is good. The method does not need to depend on complicated means such as time-consuming column chromatography or precise fractionation, the requirement for high purity can be met only through conventional extraction and crystallization operation, the technological process is simple, the method is very suitable for large-scale production, and the product purity (measured through HPLC (High Performance Liquid Chromatography)) can stably reach 98% or above.

The invention relates to a synthesis method of a branched chain type allyl alcohol compound, which comprises the following steps: under the protection of nitrogen, taking different substituted terminal alkyne and formalin as raw materials, taking metal cobalt salt and an organic ligand as catalysts, taking Hanus ester as a reducing agent, and carrying out a reaction in the presence of an organic solvent and a photosensitizer to obtain the branched chain type allyl alcohol compound. And carrying out illumination reaction to obtain the branched chain type allyl alcohol compound. According to the method, reaction raw materials and reagents are simple and easy to obtain, conditions are mild and easy to control, atom economy is high, precious metal catalysis is not needed, the substrate application range is wide, regioselectivity is high, and wide application prospects are achieved.

The invention belongs to the technical field of synthesis of 2, 3-dipicolinic acid, and relates to a catalyst for synthesizing 2, 3-dipicolinic acid as well as a preparation method and application thereof, the catalyst is prepared from a carrier, and active components and auxiliaries loaded on the carrier; the carrier is boron nitride modified aluminum oxide, the active component is palladium-cobalt bimetal, and the auxiliary agent is magnesium; the catalyst comprises the following components in percentage by mass: 0.2 wt%-3wt% of palladium, 0.5 wt%-4wt% of cobalt, 0.05 wt%-0.3 wt% of magnesium, 5wt%-15wt% of boron nitride and the balance of an aluminum oxide carrier. The catalyst is prepared by adopting an ultrasonic-assisted sol-gel method, so that high dispersion and strong interaction of active components are realized. The catalyst shows high catalytic activity, high selectivity and excellent stability in a dichloropyridine carbonylation reaction, carbon monoxide is used as a carbonyl source, the atom economy is high, and the green chemical requirement is met.