40results about How to "Facilitate large-scale synthesis" patented technology

The invention relates to a preparation method for cuprous oxide micron/nano crystal with controllable morphology, relating to the preparation method for the cuprous oxide micron/nano crystal. The invention mainly solves the technical problems of high cost and environmental pollution in the preparation process of the micron/nano cuprous oxide. The method comprises the following steps of: 1, dissolving copper salt into ultrapure water, pouring lactic acid, continuously stirring, regulating a pH value, cooling to the temperature of 25 DEG C, keeping constant volume, measuring the pH value, and obtaining solution A; 2, moving the solution A to a hydrothermal reaction kettle, sealing the reaction kettle, putting the hydrothermal reaction kettle into a drying oven, keeping the temperature, naturally cooling to a room temperature, centrifugally washing by using the ultrapure water, centrifugally washing by using anhydrous ethanol, transferring the reaction kettle onto watch glass, and drying the reaction kettle in the drying oven; and thus obtaining the cuprous oxide micron/nano crystal. The preparation method for the cuprous oxide micron/nano crystal with the controllable morphology has the advantage of simpleness and practicability, simple equipment operation, low raw material price, easy synthesis, less pollution to environment and high synthetic concentration, the problem of the cost of the morphology control and industrialized large-scale synthesis in the prior art is solved, and the industrial production is facilitated.

Methods of preparing and purifying 9-nitrominocycline and 9-aminominocycline and salts thereof used in the process of making tigecycline, are disclosed. In one embodiment, the invention is directed to a method of preparing the compound of formula 1

or a pharmaceutically acceptable salt thereof, comprising:

• (a) reacting nitric acid with the compound of formula 2,

or a salt thereof, to produce a reaction mixture comprising an intermediate; and

• (b) further reacting the intermediate to form the compound of formula 1, wherein the intermediate is isolated from the reaction mixture, the method further comprising sparging with an inert gas prior to step (a).

The invention provides a method for restoring a silver ammonia solution with ultraviolet light to prepare water-soluble silver nano-clusters. The method includes: adding an AgNO3 solution to a reaction vessel, slowly adding a NaOH solution to the vessel in oscillation, after sediment is generated, dropwise adding NH3.H2O to the vessel in oscillation till the sediment is fully dissolved, and adding redistilled water to prepare a silver ammonia stock solution with the concentration of 5.0*10<-3>M; dropwise adding carboxymethyl dextran to a weighing bottle, adding the silver ammonia stock solution in stirring, adding secondary water till volume of the solution reaches 5 to 10 times of that of the carboxymethyl dextran, stirring the solution with a magnetic stirrer for 5 to 10 minutes, and placing the solution in an exposure manner at the normal temperature under an ultraviolet lamp prior to stirring while light the solution for 2 to 4 hours. The carboxymethyl dextran is taken as a stabilizer and a reducing agent, and the water-soluble silver nano-clusters can be synthesized from the silver ammonia solution under irradiation of the ultraviolet light.

The invention discloses a method for preparing arylboronic acid neopentyl glycol ester.The method includes the steps that a mixed-type nickel (II) complex with Ni(P(OR1)3)((R2NCH2CH2NR2)C)X2 as the chemical formula serves as a catalyst, and a cross coupling reaction of phenyl chlorine substitutes and bis(neopentyl glycolato) diboron is efficiently catalyzed in potassium methoxide to prepare the arylboronic acid neopentyl glycol ester.The method is the first case that the mixed-type nickel (II) complex catalyzes the cross coupling reaction with phosphite ester and n-heterocyclic carbine as auxiliary ligands.

The invention discloses a non-uniform clustering perforation optimization method for non-homogeneous shale. The non-uniform clustering perforation optimization method comprises the steps that a plurality of shale targets are manufactured according to the reservoir shale characteristics of different well segments of shale horizontal wells, wherein the reservoir shale characteristics comprise the shale bedding inclination angle, the mechanical properties of the shale, the crack characteristics and the lithologic characteristic, and one or more reservoir shale characteristics of any two shale targets are different; and the multiple shale targets are subjected to a perforation test through multiple perforation modes and multiple perforation parameters, and the hole quality parameters, the rockpermeability and the development situation of impact cracks around a hole after perforation are detected so as to determine the influence law of different influence factors on the hole quality parameters, the rock permeability and the development situation of impact cracks around the hole; and non-uniform clustering perforation optimization of the non-homogeneous shale is conducted according to the influence law. According to the non-uniform clustering perforation optimization method, the technical problem that a non-uniform clustering perforation optimization method of the non-homogeneous shale is difficult to realize in the prior art is solved.

The invention discloses a carbon-based nanocomposite material for an electrode, and belongs to the field of preparation of metal@carbon nanocomposite materials. According to a preparation method, the carbon-based nanocomposite material for the electrode is obtained by high-temperature pyrolysis of a metal-organic skeleton compound in an inert protective atmosphere. The metal-organic skeleton compound [Ni2(L-asp)2(bpy)] is utilized as a precursor; and the carbon-based nanocomposite material with a uniform dimension is prepared through a one-step high-temperature pyrolysis process. The product obtained by the method is single in phase, very few in impurities, especially easy to collect, high in yield and beneficial to large-scale synthesis; and the microstructure of the carbon-based nanocomposite material prepared by the method has excellent properties of high stability and the like in application of the electrode material of a lithium-ion battery.

Belonging to the field of water splitting new energy technologies, the invention provides a high efficiency water splitting oxygen electrode suitable for natural water and a preparation method. In the electrode, Co-Fe hydrotalcite has a mass percentage content of 3-5%, a particle diameter of 50-00 nm, and a specific surface area of 30-50m<2>/g; the used conductive carbon black is Vulcan XC-72 type, and has a mass percentage content of 7-16%; the used titanium mesh is a plain titanium mesh with equal warp and weft wire diameter density, has a thickness of 0.2-0.5mm and a mass percentage of 79%-90%. According to the preparation method, the Co-Fe hydrotalcite, carbon black and a metal titanium mesh substrate for loading are integrated into the composite electrode. The electrode can carry a simple three-electrode system to be used for oxygen evolution reaction in natural water and neutral non-buffer solutions, including natural seawater and neutral sodium chloride solutions, etc. The preparation method is simple and is easy to realize industrial production, and has no side reaction influence.

The invention discloses a method for synthesizing fluorogold nanometer quantum dots by taking micromolecules as a stabilizer. The method is characterized by comprising the following steps: (1) preparing a SnCl2 solution which utilizes trisodium citrate as the stabilizer; and (2) synthesizing fluorogold nanometer quantum dots by taking the SnCl2 solution, an HAuCl4 solution, an H202 solution and an H3PO4 solution as raw materials and adopting a hydrothermal method. The method can be used for facilitating large-scale synthesis by adopting conventional micromolecules as the stabilizer; the synthesis period is short and only lasts for two hours, the particle size is small, and strong fluorescence can be produced.

The invention discloses a linear antibacterial oligopeptide SLAP-S25 and an application thereof. The linear antibacterial oligopeptide SLAP-S25 is an oligopeptide obtained by acetylation modificationof a nitrogen terminal and amidation modification of a carbon terminal of the oligopeptide as shown in a sequence 1 in a sequence table which is described in the specification. Experiment results showthat the linear antibacterial oligopeptide SLAP-S25 has a certain bacteriostatic effect on a variety of gram-positive and gram-negative bacteria, has good synergistic effects with antibacterial drugs(like tetracycline, vancomycin, ofloxacin and rifampicin), can restore the sensitivity of polymyxin-resistant gram-negative bacteria to polymyxin, reinforces the sensitivity of klebsiella pneumoniaeto a variety of antibacterial drugs, is free of hemolysis, has good tissue compatibility, can effectively inhibit polymyxin drug-resistance bacteria, and can treat bacteremia. The linear antibacterialoligopeptide SLAP-S25 provided by the invention has the advantages of small molecular weight, simple structure, convenient large-scale synthesis and important application values.

The invention in one embodiment is directed to a method of preparing a compound of formula 1,

or a pharmaceutically acceptable salt thereof, wherein R₁ and R₂ are each independently chosen from hydrogen, (C₁-C₆)alkyl, and cycloalkyl, R is —NR₃R₄, where R₃ and R₄ are each independently chosen from hydrogen, and (C₁-C₄)alkyl; and n ranges from 1-4, comprising:

(a) reacting a C₁-C₁₂ alkyl nitrate with a compound of formula 2,

or a salt thereof, in the presence of an acid at a concentration greater than 70% weight of acid/weight of solution, the acid being selected from the group consisting of sulfuric acid, and R₅—SO₃H wherein R₅ is C₁-C₄ alkyl optionally substituted with one or more halogen, or R₅ is C₆-C₁₀ aryl optionally substituted with one or more C₁-C₄ alkyl or halogen, to produce a reaction mixture containing a compound of formula 3 or a salt thereof;

(b) reducing the compound of formula 3 or a salt thereof to form a compound of formula 4 or a salt thereof

(c) acylating the compound of formula 4 to form a compound of formula 1; and

(d) optionally forming a pharmaceutically acceptable salt of the compound of formula 1.

The invention belongs to the technical field of preparation of covalent organic framework materials, and provides a photosensitive covalent organic framework material as well as a preparation method and application thereof. The organic monomers 4, 7-bis (4-aminophenyl)-2, 1, 3-benzothiadiazole and trialdehyde phloroglucinol are connected through a covalent bond at room temperature to form a photosensitive covalent organic framework material (COFs), and the photosensitive COFs material has an enol type structure and a ketone type structure at the same time, has excellent photosensitive property, and can generate I-type and II-type active oxygen at the same time under the irradiation of visible light. The preparation method only needs one-step simple reaction, the synthesis method is simple and convenient, the synthesis condition is mild, the consumed time is short, and large-scale synthesis is facilitated. Furthermore, the preparation method provided by the invention is easy to separate and purify, and the photosensitive COFs material can be obtained only by washing with an organic solvent.

The invention provides a soluble linear conductive polymer and a preparation method thereof. The preparation method comprises the following steps: S1, taking S-dodecyl-S'-(R, R'-dimethyl-R''-(2-thienyl) ethyl acetate) trithiocarbonate as a chain transfer agent; carrying out a reversible addition-fragmentation chain transfer polymerization reaction on methyl acrylate, 2-(Dimethylamino)ethyl methacrylate and 1, 4-dioxane under the initiation of azodiisobutyronitrile to obtain polymethylacrylic acid N, N-dimethylaminoethyl ester-b-polymethyl acrylate; and S2, adding a 3, 4-ethylenedioxythiophenen-butyl alcohol solution into the polymethylacrylic acid N, N-dimethylaminoethyl ester-b-polymethyl acrylate hydrochloric acid solution, and carrying out interfacial polymerization reaction under theaction of a catalyst to obtain the soluble linear conductive polymer. The soluble linear conductive polymer is synthesized by adopting reversible addition-fragmentation chain transfer polymerization and interfacial polymerization methods, so that the length of a flexible chain segment of the soluble linear conductive polymer is controllable.

The invention provides a bovine serum albumin-tea polyphenol molybdenum nano-composite, and belongs to the field of nano-medicine. The bovine serum albumin-tea polyphenol-molybdenum nano-composite is prepared by dissolving bovine serum albumin in water, dropwise adding a tea polyphenol aqueous solution and a molybdenum source aqueous solution, dropwise adding a sodium hydroxide aqueous solution, and reacting by adopting a biomineralization method to obtain the bovine serum albumin-tea polyphenol-molybdenum nano-composite. The invention also provides application of the bovine serum albumin-tea polyphenol molybdenum nano-composite in preparation of drugs for treating cancer cell immunogenic cell death and tumor immunotherapy. The composite provided by the invention has good biocompatibility, good dispersibility in water and good capability of triggering mouse cancer cell immunogenic cell death, and can be effectively applied to immunotherapy of tumors.

The invention relates to a method for preparing amide compounds through ionic liquid catalysis in a high-pressure environment. According to the method, ionic liquid 1-ethyl-3-methylimidazolium acetateis used as a catalyst and a solvent, oxygen is used as an oxidizing agent, and aromatic methanol or alkyl alcohol is converted into an amide compound under the conditions of high pressure and heating. The synthesis method provided by the invention has the advantages that the raw material and technical cost is low; compared with other traditional methods, the method is safe, low in toxicity, economical and environmentally friendly; and the method has few steps, is simple and convenient to operate, is beneficial to large-scale synthesis, and has important significance for synthesis of amide compounds and large-scale industrialization of preparation.