77results about How to "High reaction yield" patented technology

The application belongs to the technical field of organic synthesis, and specifically provides a preparation method of Mal-PEG2-CH2COOH, comprising the following steps: S1, reacting AEEA with maleic anhydride to generate an intermediate, wherein the intermediate is (Z)-2-(2-(N-hydroxyethyl)hydroxyethyl)carboxymethyl)maleic acid monoamide; and S2, performing ring closure reaction on the intermediate to generate Mal-PEG2-CH2COOH. According to the preparation method of the embodiment of the application, the open ring-closure step-by-step synthesis strategy is adopted, so that the harsh reaction condition of high temperature and acid is avoided, the preparation cost is reduced, the overall reaction yield is improved, and the three-waste discharge and environmental pollution are reduced.

This invention discloses a method for synthesizing cefotiam, using 7-aminocephalosporanic acid (7-ACA) as the parent nucleus and introducing a 4-dimethylaminopyridine-dimethyl carbonate composite catalytic system. The reaction is carried out in a one-pot process involving 3-position nucleophilic substitution, 7-position amidation, and simultaneous deprotection in a green mixed solvent of ionic liquid [BMIM]BF₄-water with 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazole and compound I. This method simplifies the process, improves selectivity, produces a high-purity product with stable yield, and is suitable for industrial production.

A method for preparing a substituted acrylate compound of general formula (I) is provided.

The application discloses acetoacetamide modified polyvinyl alcohol and a preparation method thereof, and the preparation method comprises the following steps: reacting p-ester and an acetoacetamide reagent at 20-80 DEG C for 1-3h in a polar solvent to generate N-acetoacetyl p-ester; then, the N-acetoacetyl p-ester is mixed with an alkaline catalyst and polyvinyl alcohol, and is added into a double-screw reaction extruder to generate N-acetoacetyl p-ester modified polyvinyl alcohol crude product; finally, the crude product is powdered, washed with methanol for three times to remove the catalyst and reaction inorganic salt, and is filtered and dried to obtain the N-acetoacetyl p-ester modified polyvinyl alcohol. The AAE-PVA prepared by the application can be used as a protective colloid for polyvinyl acetate emulsion polymerization, has better water resistance than common polyvinyl alcohol, and the water resistance, tensile strength and stability of the prepared emulsion adhesive are obviously improved. The synthesis steps of the application are simple, the safety risk is low, and the reaction yield is high.

The application provides a preparation method and application of a compound III, and belongs to the field of medicinal chemistry. The method uses compound I as a raw material, and compound III is prepared through acyl chloride and Friedel-Crafts acylation reaction in a one-pot two-step method, and a reaction formula is shown in the following formula: The synthesis method provided by the application solves many pain points of the existing synthesis method using polyphosphoric acid as a dehydrating agent, for example, the polyphosphoric acid has strong corrosion, is viscous and not easy to transfer, the reaction temperature is high, the substrate is easy to polymerize, product purification needs vacuum distillation, and there are many phosphorus-containing waste water, etc. The synthesis method has the advantages of simple operation, environmental friendliness, mild and safe reaction conditions, high reaction yield and the like, and is suitable for large-scale production.

The invention relates to a preparation method and application of a nucleating agent. The preparation method comprises the following steps: mixing solvent pure water, calcium hydroxide and fatty acid methyl ester sulfonate, and heating; dropwise adding hexahydrophthalic anhydride into the mixed solution, and after dropwise adding is completed, carrying out heat preservation reaction to obtain the calcium hexahydrophthalate. The product has excellent performance when used for thermoplastic resin such as polyolefin.

This invention discloses a lens-type ion mobility tube. An ion optical lens with radial divergence and then radial convergence of the ion beam is disposed within the ionization region of the ion mobility tube. This increases the probability of contact between the reactant ions generated by the ion source and neutral sample molecules, thereby enabling a sufficient ion-molecule reaction to generate high-abundance sample product ions and improving the detection sensitivity of the ion mobility tube. This ion mobility tube technology organically combines increasing the ion-molecule contact probability to improve the ion-molecule reaction yield with radial convergence of the ion beam to improve the ion number density, providing a novel approach to enhancing the detection sensitivity of ion mobility spectrometry. This technology does not require modification of the existing ion mobility tube structure; it can be achieved simply by changing the voltage applied between adjacent electrodes within the ionization region, facilitating its widespread application in the field of ion mobility spectrometry.

The application discloses a kind of photocontrol chiral ligand based on diarylethene, structural general formula is as shown in following formula:After the photocontrol chiral ligand based on diarylethene synthesized in the application and rhodium catalyst coordination, when catalyzing asymmetric carbon hydrogen amidation at room temperature, higher reaction yield and higher ee value can be obtained by using ligand in open loop state to catalyze, and lower reaction yield and lower ee value can be obtained by using ligand in light stable state to catalyze.The application makes up the deficiency that there is currently lack of photo-thermal bistable photocontrol catalyst in the field of photocontrol asymmetric catalysis, and widens the application of diarylethene in photocontrol asymmetric catalysis.

This invention provides a method for synthesizing quinazoline derivatives using a manganese-based catalyst. The method uses o-aminobenzyl alcohol and amide compounds as raw materials, and synthesizes quinazoline derivatives under the catalysis of a manganese catalyst with a tridentate nitrogen-phosphine ligand. This method features stable and readily available reactants, an environmentally friendly reaction process, a wide range of applicable substrates, and high functional group compatibility. Because the tridentate nitrogen-phosphine ligand significantly enhances the catalytic activity of the central manganese metal, the reaction yield reaches over 90%. This invention provides a highly atom-economical, environmentally friendly, simple, and efficient method for synthesizing quinazoline derivatives, aligning with the current trend of green chemistry and possessing significant implications for organic synthesis, medicinal chemistry, and materials science.

This invention relates to an industrial preparation method for 2-methylphenylacetic acid, comprising the following steps: under an inert solvent, 2-methylhalobenzene and malonate diester undergo a coupling reaction in the presence of a catalyst and base A to obtain compound one; compound one is hydrolyzed and decarboxylated under the presence of base B to prepare 2-methylphenylacetic acid; the chemical structural formula of compound one is: [formula missing], where R is a C1-C8 alkyl group. Compared with existing technologies, this invention uses inexpensive raw materials, is simple to operate, can react under normal pressure, has relatively mild conditions, is safe and environmentally friendly, and is easy to industrialize.

The invention discloses a synthesis method of an FLT3 inhibitor of quinatinib dihydrochloride. According to the method disclosed by the invention, the raw material drug of the quinatinib dihydrochloride is synthesized and prepared through seven chemical reactions including Boc protecting group feeding, bromination reaction, condensation ring closing reaction, Boc protecting group removal, phosgene condensation reaction, final etherification reaction to obtain the quinatinib, and final salification. The method has the advantages of wide raw material source, low cost, simplicity in operation, high product recovery rate, easiness in industrial industrialization and the like.

The invention discloses a preparation method of N-acetyl blue and application of the prepared N-acetyl blue in fabric dyeing, and relates to the technical field of compound synthesis. According to the preparation method of the N-acetyl blue, H2SO4 and aluminum chloride are adopted as a composite catalyst to catalyze N, N-dimethyl formamide; according to the present invention, the N, N '-diacetyl blue hydrolysis reaction is performed, such that the potential barrier of the N, N'-diacetyl blue hydrolysis reaction can be reduced so as to directionally remove one acetyl in the molecule to generate the N-acetyl blue, the product with the yield of more than 53% and the purity of more than 78% can be obtained by using the preparation method, and the purity and the reaction yield are excellent.

The invention belongs to the field of organic chemical synthesis, and particularly relates to a preparation method of imino aryl compounds and intermediates. The preparation method of the intermediate comprises the following steps: carrying out selective dechlorination reaction on a compound III to obtain a compound IV, wherein the reaction formula is shown in the specification; and carrying out subsequent reaction on the intermediate compound IV to obtain the imino aryl compound. The preparation method disclosed by the invention has the advantages of high yield, high product purity and easiness in industrial production.

The application discloses a macrocyclic chelator and a synthesis method, and belongs to the field of nuclear medicine chelators. The macrocyclic chelator is named as 6,6'-[3,10-dioxa-6,13-diaza-1,8(2,6)-dipyridinocyclotetradecane-6,13-diyl bis(methylene)]dipyridine-2-carboxylic acid. The macrocyclic chelator is synthesized in eight steps by taking 2,6-pyridine dimethanol as a raw material. The application successfully adopts a new method to realize an important breakthrough in a ring-closing step, and ingeniously introduces an amino group protection in multiple steps needing purification, so that a high-purity crystal Macropa analogue new chelator product is finally obtained. The application provides a new idea for subsequent synthesis of Ac-225 new chelator molecules, and to some extent, makes up for the shortcomings of existing chelator molecules.

The invention relates to the technical field of pesticides and herbicides, and discloses a preparation method of halauxifen-methyl as shown in a formula (I). The preparation process of the halauxifen-methyl and the key intermediate of the halauxifen-methyl provided based on the new intermediate compound has the obvious advantages of mild reaction conditions, low cost of raw materials and reagents, less impurity generation, high reaction yield, high product content and the like.

The application belongs to the technical field of medical intermediates, and relates to a production method of a clotrimazole intermediate (2-chlorophenyl)diphenylmethanol. In the method, 2-methyltetrahydrofuran or cyclopentyl methyl ether is used as a reaction solvent, an ethyl o-chlorobenzoate solution is added dropwise into a phenyl magnesium bromide solution with a concentration of 2.5-3.5 M under the conditions of 60-80 DEG C and inert atmosphere, the reaction is continuously carried out after the dropwise addition is completed, a water solution of a quenching agent is added after the reaction to quench, then, liquid separation is carried out, and the organic phase after the liquid separation is concentrated to obtain a crude product; the crude product is refined by using a reaction solvent and petroleum ether, and (2-chlorophenyl)diphenylmethanol is obtained. The production method can efficiently and stably produce high-quality (2-chlorophenyl)diphenylmethanol, reduces production cost and safety hazards, and can be used for large-scale industrial production.

The application discloses a preparation method of a nickel catalyst for olefin polymerization, and comprises the following steps: (1) reacting acenaphthenequinone, a water-removing agent and a substituted aniline in a first solvent under the action of a catalyst; after the reaction is completed, cooling, filtering and concentration crystallization are performed to obtain a diimine ligand; and (2) reacting the diimine ligand and a nickel salt in a second solvent; after the reaction is completed, concentration crystallization, filtering and washing are performed to obtain the nickel catalyst. The application effectively solves the problems of poor selectivity, low yield and complex post-treatment in the preparation process of the nickel catalyst, and has the advantages of a short process flow, high yield and simple post-treatment.

This invention discloses a process and reaction system for producing 8-hydroxyquinoline, belonging to the field of chemical equipment and process technology. The invention uses o-aminophenol, o-nitrophenol, and acrolein as raw materials, p-toluenesulfonic acid as a catalyst, and a benzene solvent system to prepare 8-hydroxyquinoline. This solves the problems of high waste salt content, acrolein polymerization, large footprint, and unstable product indicators in current 8-hydroxyquinoline production processes. The process for producing 8-hydroxyquinoline in this invention has the advantages of simple equipment operation, stable operation, high production efficiency, high product purity, and environmental friendliness.

The present application relates to the field of organic synthesis, in particular to a kind of preparation of flubendiamide intermediate compound I method, the method includes the following steps: compound a occurs reduction in the presence of catalyst and base and obtains compound I.The present application is by adding basic compound in the process of catalytic hydrogenation reaction, effectively 2,5-dichloro-4-(1,1,2,3,3,3-hexafluorophenoxy) nitrobenzene is reduced to only obtain 2,5-dichloro-4-(1,1,2,3,3,3-hexafluorophenoxy) aniline, and the content of dechlorination by-product is low, and the product purity is high.

This invention provides a method for the catalytic hydroboration of nitrile compounds, belonging to the field of nitrile reduction technology. The method uses nitrile compounds as substrates, molybdenum hexacarbonyl as a catalyst, and pinacolborane as a hydrogen source, with the hydroboration reaction occurring at 78-82°C for 7.5-8.5 h. The reaction utilizes molybdenum hexacarbonyl as a catalyst, which is simple and readily available, requiring no complex synthesis. Furthermore, the reaction process does not require the participation of ligands. Using pinacolborane as a hydrogen source eliminates the need for strictly nitrogen-protected experimental conditions, enabling the hydroboration of nitriles. The substrate applicability is broad, applicable not only to aromatic nitriles but also to aliphatic nitriles and even some dinitriles. The reaction process does not require solvents, making it environmentally friendly. The corresponding hydroboration product is obtained directly after the reaction without further purification, and the reaction yield is high, ranging from 84-100%.

The application relates to a preparation method of (S)-oxetan-2-methylamine and a p-toluenesulfonic acid salt thereof. By adopting a specific preparation route, the problem of poisoning of a palladium-carbon catalyst caused by residual sulfur elements is solved, and the use of explosive and highly toxic sodium azide is avoided. The process is safe and reliable, raw materials are low in price, product quality is good, chiral purity is high, and the method is suitable for industrialized scale production.

The invention relates to the field of synthesis of drug intermediates, in particular to a preparation method of 3-oxo-1-oxa-8-azaspiro [4.5] decane-8-tert-butyl formate. The preparation method comprises the following steps: carrying out condensation reaction on a compound III (4-ethoxycarbonyl methylene-1-tert-butyl piperidinecarboxylate) and methyl glycolate to generate a five-membered ring, and preparing to obtain a compound IV; according to the preparation method, tert-butyl 3-oxo-1-oxa-8-azaspiro [4.5] decane-8-formate (compound I) is prepared through a decarboxylation reaction of the compound IV, and the total yield of the reaction can reach 88.73%. The preparation method provided by the invention has the advantages of easily available raw materials, simple operation and high reaction yield.

The application discloses a synthesis method of a sulfentrazone intermediate. A compound shown in formula II is chlorinated in the presence of a solvent to synthesize a compound shown in formula I by adding a composite catalyst, wherein the composite catalyst comprises catalyst A and catalyst B in a weight ratio of 0.1-20:0.01-10; the catalyst A is one or both of a metal or a metal chloride; and the catalyst B is a compound capable of reacting with water to remove water in a reaction system. The method is simple in operation, easy to industrialize, relatively mild in reaction environment, cheap in catalyst, and high in reaction yield and product content.

The application belongs to the field of organic synthesis and particularly relates to a synthesis method of substituted silabicyclo[4.1.0]heptan-2-one derivatives. The method comprises the following steps: pyridine N-oxide mediates intramolecular radical tandem cyclization reaction of 1,6-silabenzyne compounds to obtain silabicyclo[4.1.0]heptan-2-one derivatives. The reaction condition of the application is mild and simple, only needs to add a catalytic amount of non-metal photocatalyst, does not need to add other metal catalysts and ligands; and the reaction does not need strict anhydrous and anaerobic conditions, is easy to operate, has a relatively short reaction time, the product is easy to separate and purify, and has a relatively high yield.

This invention relates to an electroactive porphyrin-based conjugated microporous polymer material, its preparation method, and its applications. The porphyrin-based conjugated microporous polymer is obtained from raw materials containing porphyrin-based monomers and aromatic amine monomers through a coupling reaction. The electroactive porphyrin-based conjugated microporous polymer material of this invention exhibits excellent electrochemical performance as an electrode material. Lithium-ion capacitors constructed using this material possess characteristics such as high specific capacitance, high energy density, fast charging rate, and long cycle life. This invention has good application potential in lightweight, high-specific-energy, fast-charging energy storage devices.

The present application relates to a kind of preparation method of STING agonist and its intermediate, overcome the low yield in prior art, two-step yield is only 7.2%, the shortcoming of poor atomic economy, the target product can be prepared only by ring closure, deprotection reaction, and reaction yield is high, can reach 82%, compared with prior art route, overall yield is increased by more than 70%, with unexpected technical effect.Moreover, the synthesis method provided by the present application has mild reaction conditions, simple and convenient operation method, not only suitable for small amount preparation in laboratory, but also suitable for industrial large-scale production.

The present application belongs to the technical field of organic synthesis, and particularly relates to a preparation method of ethyl chrysanthemate. Glycine ethyl ester hydrochloride is reacted with sodium nitrite in a dispersion system containing organic mixed solvents to obtain a diazo ethyl acetate dispersion liquid, which is then mixed with an octacarbene and reacted under the catalysis of an organic amine catalyst to generate ethyl chrysanthemate. After the reaction is completed, the target product ethyl chrysanthemate is purified, and the organic mixed solvents collected in the purification process are recycled to step (1). The present application adopts mixed solvents such as methyl tert-amyl ether methyl ether, petroleum ether and n-hexane, and the diazotization yield reaches 96%. At the same time, an organic amine catalyst is adopted, and the cyclization yield reaches 88%. The new preparation method of ethyl chrysanthemate of the present application has significant advantages in yield and quality, and contributes a new solution to the development of the health insecticide industry and the anti-new coronavirus pharmaceutical industry.

The present application relates to the technical field of mesotrione, and particularly relates to a preparation method of mesotrione intermediate, which comprises the following steps: (1) a first reaction of a compound shown in formula (II) and sodium thiomethoxide in the presence of a first solvent to obtain a compound shown in formula (III); (2) a second reaction of the compound shown in formula (III) and hydrogen peroxide in the presence of a second solvent under the action of a catalyst to obtain a compound shown in formula (IV); (3) a third reaction of the compound shown in formula (IV) and acid liquor to obtain mesotrione intermediate shown in formula (I); wherein R1 is selected from F, Cl, Br or I; and R2 is selected from C1-C4 alkyl or aromatic group. The method can effectively improve the purity and yield of mesotrione intermediate.

The invention provides a synthetic method of a deuterated naphthalene borate compound, which comprises the steps of converting a brominated naphthalene compound into a chlorinated naphthalene compound and then carrying out deuteration, so that the generation of an isomeride is avoided, the yield of the deuteration step reaches more than 85%, the yield is improved, the deuteration cost can be effectively reduced, and the product purity reaches more than 99%. The method is suitable for industrial production.

The application discloses a composite catalyst and a preparation method and application thereof. The composite catalyst comprises iridium and a nitrogen-containing porous organic polymer. The iridium is loaded in the nitrogen-containing porous organic polymer. The nitrogen-containing porous organic polymer is a random copolymer, and a general structure formula is shown as formula I: wherein m and n represent molar amounts of monomers, a molar ratio of m and n is 1:(0-100); R 1 and R 2 are each independently selected from hydrogen, halogen, cyano, amino, C 2～6 alkenyl, C 2～6 alkynyl, C 1～14 alkyl, C 1～6 alkoxy, C 6～14 aryl, C 3～10 heteroaryl containing 1-3 heteroatoms selected from N, O and S. The composite catalyst provided by the application has a large specific surface area, contains a multi-stage pore structure, can efficiently catalyze a silicon-hydrogen addition, has good cyclic catalytic performance, and exhibits excellent activity and regioselectivity, and a reaction yield is high.