663 results about "Atom economy" patented technology

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 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 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 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 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.

The invention discloses a 3-imido-4, 5-diaryl boron oxygen heterocyclic ring onium salt derivative as well as a preparation method and application of the 3-imido-4, 5-diaryl boron oxygen heterocyclic ring onium salt derivative. The 3-imido-4, 5-diaryl boron oxygen heterocycle onium salt derivative is prepared by taking acetylenic ketone potassium fluoborate, organic amine and 2-(trimethylsilyl) phenyl trifluoromethanesulfonate as raw materials, inorganic alkali and a weak acid buffer as accelerators and water and acetonitrile as solvents through a one-pot two-step reaction, and the compound can be used for preparing organic fluorescent materials, such as organic fluorescent materials, organic fluorescent materials, organic fluorescent materials, organic fluorescent materials, organic fluorescent materials and organic fluorescent materials. The compound has obvious aggregation-induced emission (AIE) property, high quantum yield and wider fluorescence range. The target product is prepared with high atom economy reaction and high yield, and the method has the advantages of cheap and easily available raw materials, mild reaction conditions, short synthetic route, wide universal range of substrates and the like.

The invention belongs to the technical field of organic synthesis, and discloses a preparation method of a 3-alkylindole compound, which comprises the following steps: in an inert atmosphere, reacting a reaction solution mixed with an indole compound, an allyl alcohol compound, a catalyst Mn-1 and alkali at 110-150 DEG C for 12-24 hours to obtain the 3-alkylindole compound. Mn (CO) 5Br is used as a transition metal and complexed with a PNP pincerlike manganese complex to obtain the Mn-1 catalyst, the 3-alkylindole compound is obtained under the catalysis of the catalyst, allyl alcohol can be aryl allyl alcohol or aliphatic allyl alcohol, a substituent group on an indole ring can be an electron withdrawing group, the application range of a substrate is wide, meanwhile, the selection range of alkali or a solvent is wide, and the 3-alkylindole compound is suitable for industrial production. The method has the advantages of high atom economy, environment friendliness, high safety and the like.

The invention discloses a method for synthesizing a benzodithiepinone derivative through metal-free catalysis, and belongs to the field of organic synthesis. According to the method, benzo disulfonylphenol ketone and alkyne are taken as raw materials, a dual-catalysis system composed of triethylene diamine and bis (diphenylphosphine) methane is adopted, a heating reaction is performed in a 1, 4-dioxane solvent, and the target seven-membered sulfur heterocycle (benzo [e] [1, 4] dithiepin-5-ketone compound) is obtained through separation and purification. According to the method, the problem of regioselective sulfuration of alkyne is effectively solved through a synergistic catalysis mechanism of organic amine and organic phosphine, and high-precision cyclization reaction of benzobissulfonylphenol ketone and alkyne is realized. The process is mild in reaction condition, free of inert gas protection, simple and convenient to operate and good in functional group tolerance, the atom economy can reach 100%, and an efficient and practical synthesis way is provided for construction of the benzo [e] [1, 4] dithiepin-5-ketone compound with a novel structure.

The application discloses a mass transfer enhanced gas-liquid reactor, which is characterized in that a feeding inlet and a tail gas outlet are arranged on a reactor shell, and a discharging outlet is arranged at the bottom; a stirring device comprises at least one group of stirring paddles arranged in the reactor shell; a gas distribution device is fixedly connected in the reactor shell and comprises an outer cover with an upper opening and a lower opening and a gas distributor sleeved in the outer cover, a gas-liquid passage with an annular cross section is formed between the outer cover and the gas distributor, a longitudinal section of the gas-liquid passage is S-shaped, a gas distribution hole is arranged on the side, and a gas inlet pipe is communicated with the gas distribution hole. The mass transfer enhanced gas-liquid reactor has the advantages of promoting the dissolution and transmission of gas, greatly improving the gas atom economy, saving energy, uniform stirring, complete fermentation, fast reaction speed and the like.

The invention discloses a preparation method and application of a double-selenium arylamine compound. The preparation method comprises the following steps: mixing a compound shown as a formula I, a compound shown as a formula II, a copper catalyst, an oxidizing agent and a solvent for reaction to obtain a compound shown as a formula III. The bis-selenium arylamine compound is prepared from the compound shown in the formula I and the compound shown in the formula II as raw materials through a one-step method, synthesis steps are simple, the raw materials are non-toxic, low in price and easy to obtain, and the synthesis method has the advantages of being good in functional group compatibility, high in atom economy and high in yield.

The invention discloses tetraacetyl dicyclopropyl hexaazaisowurtzitane, a preparation method thereof and a synthesis method of HNIW, and belongs to the technical field of chemical synthesis. The tetraacetyl dicyclopropyl hexaazaisowurtzitane disclosed by the invention is a novel hexaazaisowurtzitane derivative, and the preparation method of the tetraacetyl dicyclopropyl hexaazaisowurtzitane has the advantages of short reaction steps, simplicity in operation, easily available raw materials and industrial application potential. The tetraacetyl dicyclopropyl hexaazaisowurtzitane disclosed by the invention can be used for synthesizing hexanitrohexaazaisowurtzitane (HNIW) in one step through nitration, so that the synthesis process is simplified, and the production cost is reduced; the specific gravity of the leaving group cyclopropyl in the cyclopropylamine raw material is small, the atom economy is good, the utilization rate of the raw material is high, waste discharge is reduced, and the method conforms to the environmental protection concept of green economy.

The application discloses a kind of S-delta-substituted caprolactam chemical / enzyme series preparation method, and the specific preparation method is: 1-substituted high allyl amine occurs dynamic kinetic resolution reaction with acrylic ester compound under the catalysis of alkaline protease (special treatment) and generates S-acryl (1-substituted high allyl) amine, then the product occurs intramolecular olefin metathesis under the catalysis of Grubbs reagent and finally generates S-delta-substituted caprolactam shown in formula (1), wherein, substituent R is phenyl, halogenated phenyl or C2-C12 alkyl.The application has mild reaction condition, is conducive to reducing the equipment requirement of preparation process, improves synthesis safety and economy;Secondly, the reaction course of the method is simple, and single configuration S-delta-substituted caprolactam can be obtained by one-pot reaction, with very high atom economy.

The invention relates to a sulfur-containing tryptophan cyclic peptide compound as well as a synthesis method and application thereof. The synthesis method comprises the following steps: carrying out electrolytic reaction on a tryptophan peptide compound with a structure as shown in a formula I or a stereoisomer thereof and a thiosulfonate compound with a structure as shown in a formula II to obtain the sulfur-containing tryptophan cyclic peptide compound with a structure as shown in a formula III or a stereoisomer thereof. The sulfur-containing tryptophan cyclic peptide compound can be obtained by directly electrolyzing the tryptophan peptide compound by adopting an electrochemical method, so that the use of a transition metal catalyst and stoichiometric alkali is avoided, the generation of chemical wastes is avoided, and the realization of atom economy is facilitated. The method has the advantages of simple operation, high product purity, easy purification, high efficiency and yield, low production cost, mild reaction conditions, no need of inert gas protection, greener reaction system, environmental protection, safety, economy, energy saving and environmental protection, and is more conducive to realization of industrial production.

The invention belongs to the technical field of medicine synthesis processes, and particularly relates to a preparation method of high-yield and high-purity tandospirone citrate. According to the method, pyrimido piperazine quaternary ammonium salt and isoindoledione are used as raw materials, a toluene and n-butanol and / or n-amyl alcohol mixed solvent is used as a solvent, tandospirone can be generated under the alkaline condition without adding a phase transfer catalyst, after acid adjustment extraction and specific organic solvent reverse phase impurity removal, a water phase is adjusted to be alkaline, and the tandospirone is obtained. And extracting with toluene, and adding a citric acid ethanol solution to directly separate out a citric acid tandospirone solid. The preparation process disclosed by the invention has a very good impurity removal effect, and the obtained tandospirone citrate is high in purity, high in process yield, good in atom economy and low in output of three wastes.

The application discloses a preparation method of a phenylacetic acid compound, and particularly, the application uses a substituted or unsubstituted aromatic hydrocarbon as a starting material, and under the action of a palladium catalyst (such as palladium acetate, palladium on carbon, palladium chloride, tetra-triphenyl palladium, etc.), the starting material is reacted with formaldehyde, HCl (aq) and CO to efficiently generate the phenylacetic acid compound. The method disclosed by the application only needs to start from the aromatic hydrocarbon, greatly reduces the difficulty and cost of obtaining the raw material, and avoids stimulating, sensitizing or toxic raw materials. Compared with the prior art, the method disclosed by the application has the advantages of simplicity and efficiency, cheap and easy-to-obtain raw materials, high atomic economy, high yield, green and pollution-free, easy industrialization and the like.

The invention discloses a preparation method of an omariglone key intermediate, which comprises the following steps: under the common catalytic action of a catalyst and a ligand, taking 4-bromo-2, 6-dimethyl fluorobenzene and hydrazine hydrate as initial raw materials, adding an additive and a solvent, and synthesizing the omariglone key intermediate under a heating condition. The preparation method provided by the invention is simple to operate, mild in reaction condition and high in atom economy, the synthesis cost is reduced, and industrial-grade large-scale production is realized.

The invention relates to a co-production preparation method of dialkyl phosphate and tetraalkyl ammonium sulfate, which comprises the following steps: trialkyl phosphate and trialkylamine are subjected to a first reaction at a first temperature, then a reaction system and excessive sulfuric acid are subjected to a second reaction at a second temperature in the presence of water, and the first temperature is higher than the second temperature; after the reaction is finished, adding an extracting agent to extract the system, and separating to obtain an organic phase and a water phase; removing the extracting agent in the organic phase to obtain dialkyl phosphate; adding tetraalkyl ammonium hydroxide into the water phase until the water phase is neutral or nearly neutral to obtain a water solution containing tetraalkyl ammonium sulfate. According to the method, the dialkyl phosphate can be obtained, the tetraalkyl ammonium sulfate salt with high added value can be obtained, the raw materials are easy to obtain, the process route is simple, the atom economy is high, the method is environment-friendly, the operation is simple, and the cost is low.