1086results about How to "The reaction steps are simple" patented technology

The invention discloses a method for preparing antithrombotic medicament apixaban. The method comprises the following steps of: obtaining a compound V by performing an amidation-cyclization two-step one-pot reaction on paranitroaniline serving as a raw material and a general purpose reagent 5-chlorine valeryl chloride under an alkaline condition; performing di-chlorination on the alpha-hydrogen of the V by using phosphorus pentachloride; performing a condensation-elimination reaction with excess morpholine to obtain a compound VI; reducing the VI into a compound VII by using sodium sulfide; performing the amidation-cyclization two-step one-pot reaction on the VII and the 5-chlorine valeryl chloride to obtain a key intermediate III; obtaining II by performing a [3+2] cyclization-elimination reaction on the III and another intermediate IV; and finally, obtaining I by performing aminolysis on the II. The method has the advantages that: process design is reasonable, expensive reagent is not used, reaction yield is high, raw material cost is low, and the method is simple and convenient to operate, has no harsh reaction condition, and is easy to perform large-scale production.

The invention provides a preparation method of a metal monatomic site catalyst. According to the synthetic strategy, a porous complex composite material coated with an acetylacetone metal salt is formed from a zinc compound and an imidazole organic ligand through coordination in a methanol solution of the acetylacetone metal salt, and then a porous carbon support doped with nonmetal heteroatomic nitrogen is formed from the imidazole organic ligand through a high-temperature pyrolytic reaction in an inert gas atmosphere, wherein metal atoms interact with surrounding nonmetal heteroatomic nitrogen and exist in the form of single atoms. The method is simple, safe, low in cost and applicable to synthesis of various noble metal and non-noble metal monatomic site catalysts, and the obtained metal monatomic site catalyst is high in metal concentration and good in heat stability, can be applied to the fields of energy, catalysis, medicine, biology and the like and has quite broad market prospect.

The invention relates to a type of antibacterial fabric and a preparing method thereof, with the preparing method comprising: adsorbing cross-linking agent to the surface of fabric containing C-H key to obtain the fabric adsorbing cross-linking agent; taking the fabric adsorbing cross-linking agent as filter cloth for filtering oxidation graphite alkene aqueous solution to obtain the fabric containing both the cross-linking agent and the oxidation graphite alkene; and employing radiation crosslinking method or heat crosslinking method to initiate the cross-linking agent upon the fabric containing both the cross-linking agent and the oxidation graphite alkene for crosslinking polymerization, thus to obtain antibacterial fabric, wherein the cross-linking agent contains more than two carbon-carbon double bonds and / or Carbon-carbon triple bonds. The method of the invention is easy to operate, consumes less amount of oxidation graphite alkene, uses less amount of time in post-treatment period, and is of low cost and suitable for large scale industrialized production. Moreover, the antibacterial fabric made in this way keeps great antibacterial performance even after repeated washing. With the cytotoxicity at Level 0 (the highest security level), the antibacterial fabric produces nearly no irritation to skin.

The invention discloses hydrophilic block polyether amino silicone oil with an amino branched chain and a preparation method thereof. The hydrophilic block polyether amino silicone oil with the amino branched chain has the following structure as shown in the specification, wherein R1 is represented by formulas shown in the specification. The preparation method comprises the following steps: carrying out mixing reaction of tetramethyl dihydro disiloxane, polysiloxane and concentrated sulfuric acid, neutralizing with anhydrous sodium carbonate, carrying out reduced pressure pumping to remove a low-boiling-point substance, and thus obtaining silicone oil with the end containing hydrogen; carrying out mixing reaction of the silicone oil with the end containing hydrogen, allyl epoxy polyether and a catalyst, and thus obtaining epoxy silicone oil; carrying out mixing reaction of the epoxy silicone oil, polyether amine and a solvent, and thus obtaining block polyether amino silicone oil; and carrying out mixing reaction of the block polyether amino silicone oil, a silane coupling agent hydrolysate and an alkali catalyst, neutralizing with glacial acetic acid, and thus obtaining the hydrophilic polyether amino silicone oil with the amino branched chain.

A method for preparing gold nanometer particles via water-phase soft template method uses water-phase soft template method, the soft group formed by carbowax (PEG) and dodecyl sodium sulfate (SDS) as soft template, mixes the water solution of chlorauric acid (HAuCl4) and said soft group, uses PEG as reducer to reduce the gold ion into gold nanometer particles in special shape and size. In reaction, the soft template and reaction period can control the size and shape of gold nanometer particles. And the reactant via high-speed eccentric treatment, deposition and washed via water to obtain the gold nanometer ball, tablet, ring or arc. The invention is characterized in narrow size and size distribution, with simple operation on shape control.

A process for separating VE, sterol and sterolester from the deodored distillate of plant oil features that the sterol is separated out by directly dynamic crystallizing, the lipase is used to convert the fatty acid in oil and the neutral oil to methylester of fatty acid, and the molecular distillation is used to separate high-purity methylester of fatty acid and VE.

The invention aims to provide an entecavir compound prepared in a novel method. The reaction procedures in the preparation method of the entecavir compound are simplified. Moreover, isopropyl is adopted as a protection agent. Since the steric hindrance can function as multiple types of directional substitution, the invention reduces the introduction of heterogeneous impurities. The reaction in multiple procedures needs no strict operating conditions. Therefore, the invention lays a foundation for industrial production.

The invention discloses a expansion-type charring agent for a flame-retardant polyolefine material and a synthesis method thereof. The synthesis method comprises the following steps: by using cyanuric chloride as an initial raw material, dropwisely adding amine containing benzene ring, phenol or thiophenol and an acid binding agent into an ice bath to obtain a monosubstituted compound; dropwisely adding aliphatic diamine or aliphatic dibasic alcohol and an acid binding agent, heating to 40-60 DEG C to react, thereby obtaining a disubstituted compound; and finally, dropwisely adding the aliphatic diamine or aliphatic dibasic alcohol and the acid binding agent, heating to 80-110 DEG C, refluxing with a condenser, cooling, washing, and drying to obtain the expansion-type charring agent containing benzene ring, triazine ring and diamino or dialkoxy group. The reaction process adopts a one-pot method, and thus, the invention has the advantages of simple technique, short reaction time and environmental protection in the preparation process; the product has the advantages of high thermal stability, favorable charring effect, low water absorptivity and favorable compatibility with alkene polymers; and after being compounded with ammonium polyphosphate (APP), the product is applicable to polyolefin materials, and has favorable flame-retardant effect.

The invention discloses a method for synthesizing dyestuff intermediate H acid by using naphthalene. In the method, the H acid is prepared by carrying out the steps of sulfonating with sulfonating agent sulfuric acid, nitrating with concentrated nitric acid, separating and neutralizing, reducing by catalytic hydrogenation, acid hydrolysis, and segregating on refined naphthalene. The H acid prepared by the method is suitable for various dyestuffs of active azo and the like, and can also be used for synthesizing medicaments. The synthesis method has the advantages of no tri-sulfonation, little waste acid amount, no alkali solution, less generated sulfur dioxide gas and inorganic salt, high yield, and reduced COD and secondary pollution of waste slag because of no iron cement generated by hydrogenation reduction.

The invention relates to an organic synthesis method, in particular to a method for synthesizing an Arbekacin and an intermediate dibekacin thereof. The method comprises the following steps of: takinga kanamycin B as initial raw material, carrying out the following processes of aldol condensation, sulfonylation, sodium iodide replacement and elimination to form double bond, de-protection under acidic condition, amino-electron reduction and final hydrogenation, thus obtaining the dibekacin; taking 3',4'-dideoxy -3',4'-didehydro-kanamycin B as raw material, using a di-tert-butyl dicarbonate toselectively protect the amidogen of 3, 2', 6', 3'' sites; subsequently using the synthesized active ester to protect the 1-site amidogen; subsequently using tri-fluoroacetic acid to remove BOC; and carrying out hydrazinolysis and catalysis and hydrogenation of platinum oxide, thus obtaining the Arbekacin. The synthesis method has the advantages of simple operation, high outcome yield, reducing thecost of raw material, optimizing the reaction route, lowering the requirements to the reaction conditions and being beneficial to industrial production.

The invention discloses a cross-linked polyquaternary ammonium salt type antibiosis monomer, a preparation method of the cross-linked polyquaternary ammonium salt type antibiosis monomer and application of the cross-linked polyquaternary ammonium salt type antibiosis monomer in dentistry repairing materials. In the preparation method, monomer bonds are connected to a dentistry resin-based material, so as to endow antibiosis property to the resin-based material. The structure general formula of the cross-linked polyquaternary ammonium salt type antibiosis monomer is shown in the specification. The preparation method comprises the following steps: 1, adding a solvent in tertiary amine substance, and adding halohydrocarbon substance for reflux reaction so as to obtain a product A, adding acyl chloride for reflux reaction by using toluene, benzene, dichloromethane or tetrahydrofuran so as to obtain quaternary ammonium salt B, and purifying the quaternary ammonium salt B; and 2, adding the acyl chloride and tertiary amine substancem by using the toluene, benzene, dichloromethane or tetrahydrofuran as the solvent, adding triethylamine as auxiliary, reacting to obtain the tertiary amine containing C=C, the tertiary amine takes acetone, metjylene dichloride and acetonitrile as the solvents, adding the halohydrocarbon for reflux reaction, and then purifying the quaternary ammonium salt monomer. In the invention, reaction steps are simple, the purity of the monomer is high, and the monomer has better compatibility and higher safety as compared with the common dentistry repairing resin monomer.

The invention discloses a cuprous oxide nanocrystalline with adjustable morphology and dimension as well as a preparation method and an application thereof. The preparation method comprises the following steps: copper hydroxide which is used as a precursor is synthesized; the pH value of the system is regulated; the system whose pH value is regulated is reduced in order to obtain cuprous oxide nanocrystalline. A surfactant is not needed to add, the cuprous oxide nanocrystalline with specific morphology and dimension can be obtained by adjusting the pH value of the reaction system, and the nanocrystalline can be used for photocatalytic degradation of organic pollutants, and the method is a rapid, simple and green preparation method of cuprous oxide nanocrystalline.

The invention belongs to the field of polymer synthesis, and relates to a high-temperature-resistant nylon PA66T material and a preparation method thereof. The nylon PA66T material is prepared from the following components in mole number: 11.00-12.32 moles of aromatic binary acid, 9.00-9.90 moles of hexane diacid, 19.20-21.34 moles of hexamethylenediamine, 0.035-0.05 mole of a nucleating agent, 0.015-0.03 mole of a catalyst and 250-300 mole of deionized water. The high-temperature-resistant nylon PA66T material provided by the invention has the advantages of light weight, high temperature resistance, high mechanical strength, superior size stability and the like, and is suitable to be applied in a high-temperature environment; and meanwhile, the high-temperature-resistant nylon PA66T material is simple in the synthesis process, is moderate in viscosity, and is suitable for industrial popularization and subsequent machine shaping.

The invention relates to a method for preparing a compound nanocrystal material for a solar cell, in particular to a novel method for synthesizing mono-dispersed multicomponent compound nanocrystals. The method can be typically applied to synthesis of chalcopyrite compounds, and comprises the following steps of: quickly injecting an oil phase solution containing a sulfur source into 180-280DEG C alcohol phase solution containing a metal source, reacting for 2 to 60 minutes, naturally cooling, and washing to obtain oil soluble multicomponent compound nanocrystal particles with narrow particle size distribution. The invention provides a two phase process for synthesizing the multicomponent compound nanocrystals for the first time. Expensive and toxic organic metals are not needed to be used in the method; and common inorganic metal salt is taken as the metal source, the reaction steps are simplified, the reaction time is greatly shortened, the production cost is reduced and the pollution is lightened, so that the method is an environment-friendly method with universality. Through the method, binary compounds, tertiary compounds, quaternary compounds and even penta-compounds can be synthesized.

The invention relates to a levocarnitine compound and a new preparation method thereof. 4-chloracetyl ethyl acetate serving as an initiative raw material is reacted with trimethylamine to generate the levocarnitine compound by using L-tartaric acid modified Ni-B / SiO2 as a catalyst in the presence of sodium hydroxide. The new preparation method has simple reaction steps, obviously lowers the cost and is more suitable for industrialized production.

The invention discloses a phosphorous and nitrogenous UV-cured flame retardant and a preparation method thereof. According to the invention, phosphorus and nitrogen compound precursor with high phosphorus content is synthesized by using raw materials of alcamines compound, aldehydes compound, and dialkyl phosphite through Kabachnik-Fields reaction; a light-cured monomer containing phosphorus and nitrogen elements is prepared through substitution / esterification reaction of the precursor with (methyl) acryloyl chloride or (methyl) propenoic acid by utilizing active hydroxy of the precursor; the monomer is used as reaction type flame retardant to be applied to light-cured resin matrix, and can curve rapidly with matrix under UV lighting to form a flame-retarded light-cured material which not only has good flame retardant property, but also can reduce the transfer and loss of the flame retardant in the using process. Compared with a conventional additive flame retardant, the compatibility of the flame retardant and the macromolecule matrix is also increased, and the duration of the flame retardant property of the material can be guaranteed.

The invention provides a lithium ion battery aqueous adhesive as well as a preparation method and a lithium ion battery electrode piece thereof. The lithium ion battery aqueous adhesive has a structure of formula I as shown in the specification. By modifying hydroxyl in a water-soluble polymer repetitive unit group, purposes of introducing a flexible side chain polarity group with a polarity anion group and improving the polarity of a polymer and a current collector can be achieved, so that the adhesive force can be improved, in addition, the flexibility of the polymer can be improved, an electrode piece with good flexibility can be manufactured, and furthermore the electrode piece has high primary coulombic efficiency. The aqueous adhesive provided by the invention is simple in preparation method, gentle in condition, easy in raw material obtaining and applicable to popularization and application.

The invention pertains to the technical field of nano-materials and new energy materials, more particularly relates to a preparation method of nano spinel lithium titanate; the preparation method comprises the steps that: titanium dioxide, metatitanic acid or titanate reacts with alkali liquor with the concentration of 6 mol / L to15mol / L for 6 hours to 48 hours under normal pressure and the temperature of 90 DEG C to 130 DEG C; then, reaction products are washed with water or acid and mixed with an aqueous solution containing lithium ion for ion exchange lasing for 10 minutes to 3 days under normal pressure; then the mixture is filtered to obtain a filter cake which is calcinated to obtain the spinel lithium titanate. In the invention, all reactions are basically carried out under normal temperature and normal temperature, which not only saves the energy consumption and reduces the cost of reaction equipment, but also simplifies the reaction procedures, creates mild reaction temperature, causes the reaction easy to be controlled and is beneficial to the large-scale industrialization of the preparation method.

The invention discloses a novel preparation method for synthesizing gefitinib. 3,4-dimethoxybenzoic acid (2) is taken as a raw material, and the method comprises the following steps of: nitrifying, demethylating and methylating the 3,4-dimethoxybenzoic acid (2) to prepare an intermediate of 2-nitryl-4-methoxy-5-methyl-hydroxybenzoate (5); reacting the intermediate with 4-(3-bromopropyl) morpholine, and introducing an alkyl side chain to prepare an intermediate 6; reducing nitryl, and performing ring formation with methanamide to construct a quinoline matrix ring 8; halogenating 4-carbonyl by using the compound 8 under the action of thionyl chloride to generate an intermediate 9; and reacting with halogen substituted aromatic amine 3-chloro4-fluoroaniline to obtain the target product of gefitinib (1). In the method, the selected initial raw material is low in cost, the synthesizing route is simplified, and the raw material utilization rate and the total yield are greatly improved. The intermediates obtained in the reactions are mostly purified by a re-crystallization method, or directly subjected to the next reaction, so the yield is high, a few three wastes are generated in the reaction process, the cost is low and the method is favorable for industrial production.

The invention belongs to the field of polymer nylon synthesis and relates to a low-water absorption biological nylon material PA610T and a preparation method thereof. The low-water absorption biological nylon material PA610T is prepared from 28-30 parts by weight of aromatic diacid, 32-34 parts by weight of sebacic acid, 38-38.5 parts by weight of hexanediamine, 0.1-0.3 parts by weight of a nucleating agent, 0.0003-0.0005 parts by weight of a catalyst and 30-50 parts by weight of deionized water. The low-water absorption biological nylon material PA610T has good fluidity and more ideal mechanical properties. Nylon prepared from the low-water absorption biological nylon material PA610T has water absorbency far lower than that of common nylon. The low-water absorption biological nylon material PA610T greatly widens a nylon application field.

The invention provides a preparation method of trifluoro methanesulfonic anhydride. The method comprises the following steps of: firstly reacting trifluoro methanesulphonyl fluoride with alkali metal hydroxide to prepare trifluoro mesylate, purifying trifluoro mesylate by recrystallization by utilizing an organic solvent, reacting trifluoro methane sulfonyl chloride with trifluoro mesylate to generate a trifluoro methanesulfonic anhydride crude product, and finally purifying trifluoro methanesulfonic anhydride by atmospheric distillation. The preparation method of trifluoro methanesulfonic anhydride can be used for not only effectively simplifying reaction steps so that the operation process is simple and convenient and the operation is safe, but also avoiding byproducts generated in the process of the traditional method for producing trifluoro methanesulfonic anhydride, and effectively reducing the contents of F<-> and SO4<2-> in the product; by utilizing recrystallization, atmospheric distillation and other methods for purification, the product purity is up to 99.5%; and more importantly, the yield of anhydride is greatly increased and raised to 88% from original 60%.

The invention relates to polymetalcarbosilane, and a preparation method and an application thereof. The structural formula of the polymetalcarbosilane is shown in the specification. In the formula, R is a methyl group, an ethyl group, a propyl group, a vinyl group, a chloromethyl group, a phenyl group or a phenylethyl group; M is Ti, Zr or Hf; and m is an integer not less than 1, n is an integer not less than 0, and Cp1 and Cp2 respectively represent a cyclopentadienyl group or a substituted cyclopentadienyl group. The method for generating polymetalcarbosilane through catalyzing an organosilane addition polymerization reaction by metallocene has the advantages of adjustability of the content of metals in polymer, simple reaction step, mild reaction conditions and low preparation cost. The polymetalcarbosilane undergoes heat treatment at above 1100DEG C in inert atmosphere to form highly pure SiC.MC diphase ceramic.

The invention relates to a method for preparing imatinib, which comprises the following steps of: with a compound N-(5-Amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidineamine shown as the structural formula (II) and a compound 4-[(4-Methylpiperazin-l-yl)methyl]benzoic acid shown as the structural formula (III) as initial raw materials, dropwise adding phosphite ester at 50-90 DEG C for 1-2 hours inthe presence of a catalyst in an organic solvent; and continuously insulating and reacting at 50-90 DEG C to obtain the compound imatinib shown as the structural formula (I). The organic solvent is N,N-dimethylformamide, N,N-dimethylacetylamide or N-methylpyrrolidone. The catalyst is pyridine; and the phosphite ester is trimethyl phosphate, triethyl phosphate or triphenyl phosphate. The technical scheme of the invention has the advantages of simple reaction step, easy control of reaction, short production cycle, low toxicity of used raw materials, less pollution to the environment and higher product quality, and the yield can reach 95 percent, and the purity reaches 99.5 percent.

The invention relates to the field of natural medicine, in particular to a method for preparing C20 position dehydroxylation dammarane type rare ginsenoside and aglycone thereof. The method for preparing the C20 position dehydroxylation dammarane type rare ginsenoside and the aglycone thereof is achieved by combining multiple means of semi-synthesis preparation, chromatogram separation and purification and the like. The method is characterized in that ginsenoside Rg2, Rh1, Rg3, Rs3 and Rh2, protopanoxadiol and protopanaxatriol are used as raw materials, one-step dehydration reaction is performed under the acidic condition, C20 position hydroxyl is removed to generate double bond isomerous series C20 position dehydroxylation dammarane type rare ginsenoside and the aglycone thereof, a liquid phase is prepared to enrich a target compound, and the target compound is concentrated and freeze-dried to obtain the C20 position dehydroxylation dammarane type rare ginsenoside and the aglycone thereof. According to the method, raw materials are easy to obtain, the reaction steps are simple, and the preparation cost is low.

The invention relates to the field of medical chemical engineering, in particular to a synthesis method of medical midbodies of para-hydroxybenzoic acetone and ortho-hydroxybenzoic acetone. The method comprises the following steps: adding para-methoxybenzoic acetone or ortho-methoxybenzoic acetone to solvent; adding an acidolysis agent for acidolysis refluence; concentrating after a reaction; adding water into concentrate for dissolution; using ethyl acetate to extract; and concentrating and rectifying an extracting solution. The invention has easily obtainable raw materials, mild reaction conditions, simple reaction procedures, high product content larger than 99 percent, product yield larger than 70 percent and low production cost and is suitable for industrialized mass production.

The invention provides a levamlodipine compound prepared in a novel method, which comprises the following steps: producing D-(plus)-levamlodipine camphorate through reaction of amlodipine and D-(plus)-camphanic acid, producing levamlodipine under the effect of sodium hydroxide, and producing the levamlodipine compound through salt forming reaction of the levamlodipine and benzenesulfonic acid. The method adopts a completely novel split reagent D-(plus)-camphanic acid, simplifies reaction procedures and is more suitable for industrial production. Moreover, the method has the advantage of high yield.

The invention discloses a rubber composite material of waste cotton material-based nano-microcrystalline cellulose and a preparation method of the rubber composite material. The method comprises the following steps: stirring natural rubber latex, adding cotton nano-microcrystalline cellulose to the natural rubber latex, stirring and mixing, so as to obtain a cotton nano-microcrystalline cellulose / natural rubber mixture; laying, carrying out demulsification coprecipitation, washing participation, and drying until the weight is constant, so as to obtain a solid cotton nano-microcrystalline cellulose / natural rubber mixture; and mixing with white carbon black, so as to obtain the required product. The nano-microcrystalline cellulose disclosed by the invention can be used as a novel reinforcing material for rubber, and has the characteristics of renewability, small density, high strength, biodegradability, biocompatibility, liquid crystalline property and the like; the preparation method is simple and convenient; the raw materials are cheap and available; the reinforcing effect of the cotton nano-microcrystalline cellulose on the rubber is superior to that of the white carbon black; the mechanical property of the rubber is well improved; and the nano-microcrystalline cellulose / white carbon black / rubber composite material can be applied to manufacturing of various vulcanized rubber products.

The invention provides a method for synthesizing a nano selenium material and relates to the application technology of selenium resources. The method includes the following steps: in an environment with a temperature of 0+ / -1 DEG C, mixing an ethanol solution of sodium borohydride with selenium powder while stirring the mixture, adding a mixture composed of sugar, lautyltrethylammonium bromide and diethyldiisopropylammonium bromide in the mixture, and then obtaining a mixture system; increasing the temperature of the mixture system to 20-60 DEG C under a stirring condition for a reaction, obtaining a precipitate after the reaction is completed, conducting suction filtration and then calcinating the precipitate at 450-550 DEG C to obtain the nano selenium material. Compared with a traditional synthesis method, the method has simple and little reaction steps, raw materials are easy to obtain, solid waste is little, the corrosivity is low, and the method is environmentally friendly and is suitable for mass production.

The invention discloses a method utilizing acidic ionic liquid in catalyzing and synthesizing diphenolic acid and / or diphenolic acid ester. The method comprises heating and stirring 1-100 parts of the acidic ionic liquid, 1-200 parts of levulinic acid and 1-500 parts of phenol for 5-60 hours' reaction under the protection of nitrogen to obtain the diphenolic acid; and continuously adding alcohols into the reacted mixture, stirring and heating the mixture to obtain the corresponding diphenolic acid ester. The acidic ionic liquid utilized in the method is sulfonic acid ion liquid including tertiary amine base monokaryon sulfonic acid ion liquid, imidazolyl monokaryon sulfonic acid ion liquid, pyridyl monokaryon sulfonic acid ion liquid, ditertiary amine base dikaryon sulfonic acid ion liquid, diimidazolyl dikaryon sulfonic acid ion liquid or dipyridyl monokaryon sulfonic acid ion liquid. The method successfully enables the acidic ionic liquid to serve as a catalytic agent to prepare the diphenolic acid and / or the diphenolic acid ester and is simple in preparation process and high in yield. According to the method, the separation of the catalytic agent and the reaction substrate is achieved through a solvent extraction method, and the catalytic agent can be repeatedly used and has no significant inactivation.