286results about How to "Efficient synthesis method" patented technology

The invention provides a metal organic frameworks-mesoporous silica composite material which is prepared by hydrothermal reaction compounding of metal organic frameworks and a mesoporous silica material, and further comprises a preparation method and application of the metal organic frameworks-mesoporous silica composite material. According to the preparation method and the application of the metal organic frameworks-mesoporous silica composite material, a material which is large in specific surface area and high in crystal form degree, carbon dioxide adsorbability and selectivity is obtained through a certain interaction between the surface of mesoporous silica and the metal organic frameworks, and the thermal stability of the material is superior to that of a pure MOFs constituting the composite material, and the synthetic method of the material is simple, efficient, good in repeatability and relatively low in cost.

The invention relates to a synthesis method of surface etched polyorthoester-polyamide copolymer (POEAd), a delivery carrier thereof and a controlled-release composition containing an active agent, which belongs to the technical field of polymer carriers and slow-release and controlled-release materials. The pharmaceutical composition can be a locally controllable delivery or injectable preparation applied to the active agent.

The invention discloses a lead coordination polymer as well as a preparation method and application thereof and belongs to the technical field of coordination compound preparation. The lead coordination polymer is prepared by taking (4,4'-(2,1,3-benzothiadiazole-4,7-diyl)-dibenzoic acid) as a ligand and enabling the ligand to react with soluble salt of Pb<2+>; a chemical formula of the lead coordination polymer is as follows: [Pb(H2L)(DMF)]n; a repeating unit contains one Pb<2+>, one (4,4'-(2,1,3-benzothiadiazole-4,7-diyl)-dibenzoic acid) anion and one coordinated DMF (Dimethyl Formamide) molecule. An experiment result shows that the lead coordination polymer prepared by the method has the advantages of good fluorescence performance and good thermal stability, and has important applicationvalue in the fields including color displays, fluorescence labels and the like.

The invention discloses a multifunctional ultrasonic microwave collaborative chemical reactor and a method for preparing a nano semiconductor chalcogenide by using the same. The multifunctional ultrasonic microwave collaborative chemical reactor comprises an ultrasonic generator, a microwave generator, a temperature / time / power display control device, a reaction vessel, a condensing device, a microwave resonator, a microwave shielding device, an air exhausting and air feeding device, and a reaction vessel supporting and lifting device. The chemical reactor has the advantages of uniform vibration, consistent action stressed by all the points in a sample medium, many varieties of selectable extraction solvents, wide range of targets, reduction of the binding force of the targets and sample substrates; accelerated process of the targets from solid phase to solvent phase, large processed sample amount and the like. The chemical reactor can overcome the phenomenon of overheat charring, and can obtain more uniform and better-quality products than single microwave reaction. The chemical reactor has wide application prospect in the fields of chemistry and chemical industry, pharmacy, materials, energy sources, food processing and the like.

The invention discloses a biological synthesis method for a spherical silver nanoparticle. The biological synthesis method includes the steps: preparing mango peel extracting solution; preparing desmodium extracting solution; performing mixture reaction: mixing the mango peel extracting solution, the desmodium extracting solution and 0.5mM silver nitrate solution accounting for 9-10 times of the weight of the mango peel extracting solution and the desmodium extracting solution, adjusting a pH (potential of hydrogen) value of the silver nitrate solution to be 8.0, and reacting the solution for 12-15min at the temperature of 50-55 DEG C. According to the synthesis method, low temperature is needed, the pH is neutral, and the prepared silver nanoparticle is fine in dispersing performance, minimal in particle size, extremely narrow in distribution range, excellent in antibacterial effect and spherical or approximately spherical.

The invention relates to a method for preparing a polycarboxylate superplasticizer by carrying out graft copolymerization on acrylic ester polymer and fatty acid vinyl ester. According to the method for preparing the polycarboxylate superplasticizer by carrying out graft copolymerization on the acrylic ester polymer and fatty acid vinyl ester, acrylic ester polymer and fatty acid vinyl ester are taken as main reaction raw materials, polymerization is carried out firstly, then grafting is carried out and then alcoholysis and hydrolysis are carried out to prepare the polycarboxylate superplasticizer grafted and polymerized with the acrylic polymer and fatty acid vinyl ester, namely acrylic ester is taken as a reaction monomer, polymerization is carried out under the actions of an initiating agent and a molecular weight regulating agent, then graft polymerization is carried out with the fatty acid vinyl ester to obtain a graft copolymer with the acrylic ester polymer as a main chain and polyvinyl ester fatty acid as a side chain, and finally alcoholysis and hydrolysis are carried out on the graft copolymer. The method for preparing the polycarboxylate superplasticizer by carrying out graft copolymerization on the acrylic ester polymer and fatty acid vinyl ester has the advantages that a process is simple and easy to control, cost is low, environmental protection is realized, no pollution is produced, the fatty acid vinyl ester is used for replacing the existing polycarboxylate superplasticizer, and diversification of raw materials is enriched; and the prepared superplasticizer has good cement paste fluidity and holding capability and shows good cement adaptability and concrete application property.

A synthesis method of a compound used to form a self-assembled monolayer used in a semiconductor component is provided. A method includes a first step of replacing a terminal halogen of an ω-haloalk-1-ene with a compound having at least one aromatic group, and a second step of hydrosilylating the reaction product of the first step. Reaction products of the first step include octadec-17-enyloxybenzene, 4-octadec-17″-enyloxy-1,1′-biphenyl, 2-heptadec-16′-enylthiophene, and 2-octadec-17′-enylthiophene. Monolayers provided include 18-phenoxyoctadecyl)trichlorosilane, [18-(1′,1″-biphenyl-4′-yloxy)octadecyl]trichlorosilane, (17-thien-2′-ylheptadecyl)trichlorosilane, (18-thien-2′-yloctadecyl)trichlorosilane, and 4-(18′-trichlorosilyloctadecyloxy)benzonitrile. An organic field effect transistor having monolayers according to embodiments of the invention is provided.

The invention discloses a method for synthesizing aromatic aldehyde, aromatic ketone and aromatic ester through catalytically oxidizing an alkyl aromatic compound by iron, and belongs to the technical field of catalytic synthesis. According to the method, a low-cost and environment-friendly iron catalyst is used under a normal pressure; under the action of hydrogen and silicon reagents serving as an accelerant and an oxidant, a side chain of an aromatic hydrocarbon is oxidized into a carbonyl group for generating the corresponding aromatic aldehyde, aromatic ketone and aromatic ester. The method for preparing the aromatic aldehyde, the aromatic ketone and the aromatic ester through a catalytic oxidation reaction, which is provided by the invention, has numerous advantages that a catalyst, reaction raw materials, the oxidant and a silicon reagent are wide in sources and good in stability and is low-cost and environment-friendly; the alkyl aromatic compound is metered to participate in a reaction; the reaction condition is mild; the compatibility of functional groups is good; the scope of application is wide; the reaction selectivity is good; in an optimized reaction condition, the separation yield of a target product can be up to approximately 95 percent.

The invention relates to a synthesis method of a cyclic orthoester monomer containing diamino, which belongs to the technical field of biological medicine and organic chemistry. The monomer is 4, 4'-dimethylene oxygen-di-(2-aminoethoxy-2-R-1, 3-dioxolane), and is a novel polyorthodester monomer, wherein R is hydrogen or methyl. The synthesis method of the orthoester monomer comprises the steps that dimeric glycerin is used as a raw material, and reacts with trimethyl orthoester in the presence of an acid catalyst; ester exchange reaction is carried out on an acquired product and 2-trifluoro acetamido ethanol in the presence of a catalyst to acquire a precursor compound of the monomer; and finally, a trifluoroacetyl protective group is removed from the precursor compound in an alkaline solution to acquire the cyclic orthoester monomer containing diamino. According to the synthesis method provided by the invention, the raw material can be easily acquired; the synthesis method is simple and economic, and is suitable for industrialized production; and the monomer is stable at room temperature, and can be used for the preparation and the application development of a novel polyorthodester polymer biomaterial.

The invention discloses the synthesis of poly lactic acid by microwave radiation melt polycondensation method which comprises, (1) placing L-lactic acid on auxiliary reaction medium, increasing the system vacuum from 0.050-0.070 Mpa to 0.080-0.099Mpa, microwave radiating 30-50 min, obtaining prepolymer (OLLA), (2) charging catalyst into the prepolymer, microwave radiating 2-5 min under normal pressure, (3) under the condition of vacuum 0.085-0.1Mpa, microwave power 500-550W, radiating 25-50min, thus obtaining polylactic acid.

The invention discloses a method for enzymatic synthesis of 1,2-diacylglycerol and a method for purifying obtained 1,2-diacylglycerol. The enzymatic synthesis method comprises the steps that vegetable oil and an organic solvent are mixed based on a molar ratio of 1 to 10-100; after stirring and emulsification, immobilized lipase with the mass accounting for 2 to 20% of the total mass of a substrate is added; after reaction for 0.5 to 6 hours at a temperature of 20 to 70 DEG C, centrifugal removing of lipase is carried out to obtain a product containing 1,2-diacylglycerol. The purification method comprises the step that two-step-crystallization-process-based purification is carried out on the product and two kinds of organic solvents. The purity of the purified 1,2-diacylglycerol can reach up to 100%. According to the method for synthetizing 1,2-diacylglycerol and the method for purifying the obtained 1,2-diacylglycerol provided by the invention, the reaction rate can increase obviously and the yield is high; the product is easy to purify and the purity is high. The methods conforming to a green chemistry concept have advantages of being high in efficiency, being fast in speed, and being convenient for industrial production.

The invention relates to a method for preparing mannose-containing derivatives capable of being used for post-polymerization modification by double-click chemistry combination. The method comprises the following steps: under the actions of propargyl bromide and acryloyl chloride respectively, preparing a compound with terminal alkyne and terminal olefin by using a Williessen ether-forming reaction; and then performing sulfydryl-alkene addition reaction on terminal olefin and sulfydryl compounds, and performing CuAAC reaction on terminal alkyne and acetyl-protected alpha-D-pyranomannose azide.Compared with the prior art, mercaptan substances with different structures are successfully combined with the alpha-D-pyranomannose azide through a mercapto-alkene addition reaction and GuAAC combined method for the first time, the mannose-containing derivative capable of being applied to post-polymerization modification is prepared, and the synthesis method is stable, efficient and high in yield. A considerable way is provided for obtaining a sugar-containing homopolymer with controllable molecular weight and narrower molecular weight distribution in the later period.

The invention discloses a reduction / pH double response adriamycin prodrug and a preparation method and application thereof. The specific preparation method comprises the steps of performing a chemical reaction by using a small molecule compound 3,3'-dithio diyne butyl dipropionate (B-ss-B) endcapped with alkynyl and a compound diazide ethyl diacetal polyethyleneglycol (N3-a-PEG-a-N3) endcapped with an azide group, so as to prepare a reduction / pH double response polymer poly(SS-alt-A)n endcapped with alkynyl; and then connecting adriamycin derivatives at two ends of a polymer chain, so as to obtain the reduction / pH double response adriamycin prodrug DOX-hyd-poly(SS-alt-A)n-hyd-DOX. The reduction / pH double response water-soluble adriamycin prodrug has good biocompatibility and characteristics of controlled-release drugs, so that the reduction / pH double response water-soluble adriamycin prodrug can be used as a stimulating sensitive antitumor prodrug.

The invention discloses a method for preparing a glycopolymer through combination of ROMP polymerization and a mercapto-alkene addition reaction. The method uses a gradient organic synthesis method, combines a thiol-ene Michael addition, and prepares a norbornene derivative of a heterosaccharide monomer containing non-protective group, and the glycopolymer with controllable molecular weight and narrow molecular weight distribution width can be obtained through ring-opening metathesis polymerization (ROMP). Based on the advantage of thiol-ene Michael addition, a feasible platform and an approach are provided for preparing the heterosaccharide monomer with an ordered side-chain structure; and the heterogeneous glycopolymer prepared by an active ROMP polymerization has important guidance meaning for researching a specific identification mechanism of a sugar unit and agglutinin as well as for developing the functional glycopolymer having a special biological diagnosis function.

The invention relates to the technical field of biology, in particular to a method for biosynthesizing nano-silver through photoinduction of imperata leaf extract. The method comprises the following steps: 1) picked imperata leaves are cleaned, dried and grinded to powder; ultrapure water is added in the powder for oscillating, extracting and centrifugating to obtain supernatant; and the supernatant is frozen and dried to obtain the imperata leaf extract; and 2) the imperata leaf extract in the step 1) is taken as a reaction matrix; AgNO3 solution is added, so that the concentration of the reaction matrix in obtained mixed solution is 10-50 mg / mL, and the concentration of AgNO3 is 1-3 mM; and nano-silver particles are prepared through reaction under sunlight irradiation or LED lamp irradiation. The biosynthesizing method is safe, environment-friendly, wide in synthetic material source and fast in synthesizing speed, can finish the reaction within 90-120 minutes, and is a green, safe and efficient biosynthesizing method.

The invention provides a guanidine substituted aromatic compound modified high polymer material shown in a formula (1). The guanidine substituted aromatic compound modified high polymer material comprises a cationic high polymer skeleton and guanidine substituted aromatic compound functional groups, and the guanidine substituted aromatic compound functional groups are covalently connected to the surface of the cationic high polymer skeleton. The invention further provides a preparation method of the high polymer material and an application of the high polymer material as a nucleic acid and protein molecule transport carrier. The synthesis method has low cost and is simple; the synthesized high polymer material is low in cytotoxicity and has the good application prospect.

The invention relates to a synthetic method of a benzenesulfonate derivative and belongs to the technical field of synthesis of compounds. A compound (described in the specification) is taken as raw materials, and reaction is carried out with ethylene glycol or R2-OH to generate a compound (described in the specification), wherein R1 is selected from alkyl, H or F, and R2 is selected from allyl, propargyl or benzene. The synthetic method provided by the invention comprises the following concrete operations: adding ethylene glycol or R2-OH and dichloromethane into a reactor, adding organic alkali while stirring, then cooling to the temperature below 15 DEG C, starting to dropwise add a substance (described in the specification), after the substance is dropwise added, returning to room temperature and further stirring for 0.5-1 hour, then heating and carrying out reflux reaction for 1-2 hours, after the reflux reaction is complete, carrying out ice thawing treatment, layering, drying, and concentrating, so that the benzenesulfonate derivative product is obtained. The synthetic method provided by the invention is simple, reaction process is mild and stable, yield is high, and the obtained product is high in purity.

The invention discloses a biological synthesis method of cubic nanometer silver particles. The biological synthesis method comprises the following steps of preparing a sweet orange peel extraction solution; preparing a lotus leaf extraction solution; performing a mixed reaction which comprises taking the sweet orange peel extraction solution and the lotus leaf extraction solution to be mixed with an 8 to 10 times of weight of 0.5 mM silver nitrate solution, adjusting a pH (Potential Of Hydrogen) value of the silver nitrate solution into 9.0 and performing the reaction for 10 to 16 minutes under 52 to 60 DEG C. According to the biological synthesis method, nanometer silver particles with small particle size, narrow distribution range and regular cubic form can be produced controllably.

The present invention provides a method for preparing a 9,11beta-epoxy steroid compound represented by a formula 1. According to the method, a 9,11-double bond-21-ester steroid compound is adopted as a raw material, and reacts with a halogenating agent in a suitable organic solvent containing 70% perchloric acid to produce a 9alpha-halo-11beta-ester-21-ester steroid compound, and the 9alpha-halo-11beta-ester-21-ester steroid compound reacts with a strong base in an organic solvent to obtain the 9,11beta-epoxy steroid compound. The 9,11beta-epoxy steroid compound can be used for preparation of dexamethasone, betamethasone and series other drugs. According to the present invention, the 9,11beta-epoxy steroid compound can be prepared from the almost equimolar amount of the 9,11-double bond-21-ester steroid compound, such that the method is the synthesis method with characteristics of economy, efficiency and environmental protection.

The invention discloses a method for synthesizing 1,2-diglyceride with an enzymic method. The method comprises the steps of mixing vegetable oil with an organic solvent according to the mole ratio of 1:10 to 100, stirring, emulsifying, then adding immobilized lipase of which the mass is 2 to 20% of the total mass of substrates, reacting for 0.5 to 6 h at the temperature of 20 to 70 DEG C, and centrifuging to remove the lipase, so as to obtain a product which contains the 1,2-diglyceride. The synthetic method provided by the invention has the advantages of high yield, high efficiency, rapidity and convenience in industrial production and conforms to green chemistry, the reaction rate can be obviously increased, and the product is easy to purify.

The invention relates to a synthesis method of environment-friendly p-methyl anisole. The method includes: taking p-cresol as the raw material, using a polar solvent like water as the solvent, adopting an alkaline substance Y type zeolite as the catalyst, and adding a proper surfactant Turkey red oil as the emulsifier, and under a 130-180DEG C temperature range and other specific conditions, using environment-friendly dimethyl carbonate (DMC) as the methylation raw material to prepare p-methyl anisole. The yield is up to 96% or above, and the final product purity is up to 99% or more.

There is provided a method of synthesizing heat elimination mastic, its producing procedure comprises the following steps: providing the filled powder and the base materials of the mastic; charging the mentioned filled powder and base materials into a container while keeping the base material in the state of melting or liquidness; pressurizing and mixing the mixture to mix them uniformly. The method has the advantage of making the heat elimination mastic mix quickly and effectively.

The invention discloses a method for carbonylation synthesis of diaryl ketones through iron catalysis and belongs to the technical field of catalytic synthesis. According to the method, in a solvent alcohol or alcohol aqueous solution, and in the action of alkali, acid and iodide, an iron catalyst is added for catalyzing a direct cross-coupling reaction of an aryl halogenated compound, an aryl boron compound and a carbonyl source including haloform or carbon tetrahalide to prepare a diaryl ketone compound. The method for preparing a diaryl ketone compound through a coupling reaction is safe in carbonyl source and easy to treat and is cheap; the catalyst is available in sources and low in toxicity and is cheap; the reaction is free of ligand and good in activity; the reaction condition is mild and the selectivity is high; the substrates are available in sources and are stable; the functional groups of the substrates are good in compatibility and the substrates are wide in application range; and the reaction medium is green and can be reused. In an optimized reaction condition, the separation yield of a target product can reach 94%.

The invention discloses a synthesis method of 4-allyl-3,5-disubstituted isooxazole, and belongs to the technical field of organic synthesis. The synthesis method is characterized in that in a reactor,acetyenic ketone oxime ether substrates, 3-bromopropylene, palladium catalysts, additives and solvents are added; stirring reaction is performed at 70 to 80 DEG C; a reaction product is separated andpurified to obtain the 4-allyl-3,5-disubstituted isooxazole. The method has the advantages that a product obtained by performing Sonogashira coupling on simple and easy-to-obtain acyl chloride and alkyne, and methoxylamine hydrochloride react to obtain a series of norethisteroneoxime ether; the reaction conditions are mild; no environment pollution exists; a potential functional 4-allyl-3,5-disubstituted isooxazole compound is built. The method has innovativeness and atom economy; the conditions are mild; the operation is safe; the scale can be magnified to 5g level scale without influencingthe yield, so that potential practical values are realized.

The invention belongs to the technical field of medical material synthesis, and particularly relates to a 3-trifluoromethyl substituted pyrazole derivative and a synthesis method thereof. The derivative is prepared by mixing an aldehyde, sulfonyl hydrazide, 2-bromo-3,3,3-trifluoropropene, an alkali and an organic solvent I for reacting, or mixing a hydrazone, 2-bromo-3,3,3-trifluoropropene, an alkali and the organic solvent I for reacting. The method has high efficiency, the reaction has good adaptability to functional groups and wide adaptability to substrates, and the product yield is high.The raw materials are cheap and easily available, and the method can be amplified to 10g-level large-scale production or larger-scale production. The method is simple and safe to operate, and mild inreaction conditions. The obtained product comprises key intermediates for constructing COX-2 inhibitor Colecoxib and Mavacoxib, lung cancer inhibitor SC-560 and measles virus inhibitor AS-136, has wide applications in the fields of pesticides, medicines and materials, and has a good industrial application prospect.

In this disclosure, transition and rare earth metal-based magnetic ionic liquids (MILs) are successfully prepared in a two-step synthesis and used to extract viable bacteria from a liquid sample. The disclosed MILs are extremely hydrophobic MILs and were insoluble in aqueous solution at 0.01% (v / v). Furthermore, these MILs were miscible in a variety of polar and non-polar organic solvents. Moreover, these MILs possess low viscosity and increased magnetic susceptibility. These MILs possess unique characteristics that can have great potential uses in various chemical applications such as extraction solvents in LLE, liquid electrochromic materials (Co-based MILs), and novel reaction media for organic synthesis.

The invention discloses a method for synthesizing chiral isonucleoside analogues through asymmetric cycloaddition reaction, and belongs to the field of asymmetric synthesis in organic chemistry. Purine substituted olefin 1 and epoxy butene 2 are used as raw materials; in the presence of a palladium catalyst and a chiral diphosphine ligand SegPHOS or MeOBIPHEP, asymmetric cycloaddition reaction iscarried out to obtain a chiral isonucleoside analogue 3, dr is 1 / 1-7 / 1, the maximum enantiomeric excess ee reaches 95%, and a variety of functional group substituted chiral isonucleosides 7-11 are obtained after derivation. The method provides a simple, convenient, cheap and efficient way for synthesizing the chiral isonucleoside compound series.

The invention discloses a method for efficiently preparing nano barium sulfate with uniform particles. Soluble BaS raw ore is used as a raw material to prepare the nano barium sulfate by virtue of pretreatment, main reaction and after-treatment. The method specifically comprises the following steps: adding the raw material soluble BaS raw ore into deionized water, dissolving to obtain a 0.1 to 5 mol / L BaS solution, wherein the BaS solution is used as a reaction solution a for standby use; preparing a sulfuric acid solution with the same concentration as the reaction solution a, wherein the sulfuric acid solution is a reaction solution b which is used for the standby use; pumping the reaction solution a and the reaction solution b into a micro reactor to react at a speed of 50 to 150 ml / min, standing for 0.1 to 20 s in the micro reactor, collecting a product c at an outlet of the micro reactor, and recovering H2S gas generated in the main reaction; and centrifuging, washing and drying the product c to obtain a target object nano barium sulfate with uniform particles. The nano barium sulfate product prepared by the method has the characteristics of uniformity in size distribution, good dispersity, narrow distribution of particle size and the like, and the particle size of the product is in a range of 30 to 50 nm.

The invention relates to a preparation method of a four-position substituted chiral spirocyclic aminophosphine ligand on a pyridine ring and an application thereof. The four-position substituted chiral spirocyclic aminophosphine ligand on the pyridine ring comprises a compound shown in a formula 1, or a racemate or an optical isomer thereof, or a catalytically acceptable salt thereof, and is characterized by comprising a chiral spiroindane skeleton and a pyridyl group. The four-position substituted chiral spirocyclic aminophosphine ligand on the pyridine ring can be synthesized by using a 7-diaryl / alkylphosphine-7'-amino-1 and 1'- spiroindane compound comprising a spirocyclic skeleton as chiral original raw materials. After the four-position substituted chiral spirocyclic aminophosphine ligand on a pyridine ring and the transition metal (iridium) salt form a complex, the complex can be used for catalyzing asymmetric catalytic hydrogenation of alpha-aromatic amine to substitute lactonecompounds. By the adoption of the preparation method of the four-position substituted chiral spirocyclic aminophosphine ligand on the pyridine ring and the application thereof, extremely high catalytic activity (TON up to 5000) and enantioselectivity (up to 98% ee) are achieved, and practical value is achieved.

The invention discloses a heteronuclear ruthenium palladium bicyclic metal compound and a preparation method and an application thereof and belongs to the technical field of organic synthesis. The metal compound is easily prepared and modified, stable in heat and air, high in catalytic activity, long in life, and the like, and is capable of playing the catalytic properties of ruthenium and palladium simultaneously when an indane benzyl substitution derivative is synthesized and prepared, so as to generate the indane benzyl substitution derivative by directly reacting halogenated acetophenone and aryl benzyl alcohol and gain the high catalytic activity. The heteronuclear ruthenium palladium bicyclic metal compound prepared by the invention is characterized by simple method, strong operability and high yield. The prepared heteronuclear ruthenium palladium bicyclic metal compound is capable of catalyzing the direct reaction of the halogenated acetophenone and the aryl benzyl alcohol and has the advantages of wide oligomer range, mild conditions, high yield, high efficiency and practicability. Furthermore, cheap weak base can be applied to the reaction due to a small dosage of the catalyst.