288 results about "One-pot synthesis" patented technology

The present invention is directed to a method of making a ligand which can be used to form an ansa-metallocene. Further, the present invention is directed to a method of making the ansa-metallocene. In both methods the process steps employed to form the ligand are conducted in the presence of tetrahydrofuran, a substituted tetrahydrofuran, tetrahydropyran, a substituted tetrahydropyran or ethylene glycol dimethyl ether.

A method of homogeneously forming metal chalcogenide nanocrystals includes the steps combining a metal source, a chalcogenide source, and at least one solvent at a first temperature to form a liquid comprising assembly, and heating the assembly at a sufficient temperature to initiate nucleation to form a plurality of metal chalcogenide nanocrystals. The plurality of metal chalcogenide nanocrystals are then grown without injection of either the metal source or the chalcogenide source at a temperature at least equal to the sufficient temperature, wherein growth proceeds substantially without nucleation to form a plurality of monodisperse metal chalcogenide nanocrystals. An optional nucleation initiator can help control the final size of the monodisperse crystals. Such synthesis, without the need for precursor injection, is suitable for the industrial preparation of high-quality nanocrystals.

Dihydrophenazines and bis(dihydrophenazines) are prepared in high yield under commercially viable reaction conditions by reacting a catechol with a 1,2-diaminoaryl compound, wherein either the catechol or the 1,2-diaminoaryl compound is provided in at least 50% molar stoichiometric excess. The product may be oxidized to the corresponding phenazine, but is preferably derivatized at one or both of the 5,10-positions to form a monosubstituted or disubstituted dihydrophenazine or bis(dihydrophenazine). Most preferably, 5,10-dialkyl-5,10-dihydrophenazines are prepared starting from catechol and 1,2-diaminoaryl compound in a one pot synthesis. The products are useful as dyes, and in particular as chromophores in electrochromic systems.

An improved opiate synthesis scheme is provided. An improvement to the oxidation of oripavine and oripavine derivatives comprises the in-situ formation of the peroxacids required to oxidize the oripavine and oripavine derivatives to form an intermediate. An improvement to the reduction of the intermediate to form oxycodone and oxycodone derivatives comprises reduction utilizing a hydrogen transfer reagent. These improvements allow the production of oxycodone and oxycodone derivatives without isolation of the intermediate, providing a one-pot synthesis method.

This invention provides molecularly imprinted polymer nanoparticles compatible with biological samples, and in particular pure biological samples and a preparation method thereof. Said molecularly imprinted polymer nanoparticles have a crosslinking degree exceeding 50%, a particle diameter of 10 to 500 nm, hydrophilic polymer brushes on its surfaces and can be prepared by introducing appropriate hydrophilic macromolecular chain transfer agents into reversible addition-fragmentation chain transfer (RAFT) precipitation polymerization systems through the one-pot synthesis. The preparation method is simple, features a broad range of application and yields a pure product. The obtained hydrophilic molecularly imprinted polymer nanoparticles have prospects for a wide range of application in biological sample analysis, medical clinical immune analysis, food and environmental monitoring, biomimetic sensors, etc.

A method of forming a hybrid physically and chemically cross-linked double-network hydrogel with highly recoverable and mechanical properties in a single-pot synthesis is provided. The method comprises the steps of combining the hydrogel precursor reactants into a single pot. The hydrogel precursor reactants include water; a polysaccharide; a methacrylate monomer; an ultraviolet initiator; and a chemical crosslinker. Next the hydrogel precursor reactants are heated to a temperature higher than the melting point of the polysaccharide and this temperature is retained until the polysaccharide is in a sol state. Then the single-pot is cooled to a temperature lower than the gelation point of the polysaccharide and this temperature is retained to form a first network. Thereafter, photo-initiated polymerization of the methacrylate monomer occurs via the ultraviolet initiator to form the second network.

Disclosed are a complex oxide catalyst for dehydrogenation, a method of preparing the same, and use thereof, wherein the catalyst includes a first transition metal selected from the group consisting of gallium, vanadium, chromium, manganese, molybdenum, and zinc, a hydrogen-activating metal including at least one selected from the group consisting of Groups 8, 9, 10, and 11 elements in a periodic table, and alumina, the amount of the first transition metal being 0.1 wt % to 20 wt %, the amount of the hydrogen-activating metal being 0.01 wt % to 2 wt %, based on the amount of the alumina, the first transition metal being loaded on the alumina, and the hydrogen-activating metal being surrounded by the alumina.

A process is provided for the semi-synthesis of taxane intermediates useful in the preparation of paclitaxel and docetaxel, in particular, the semi-synthesis of protected taxane intermediate in a one pot reaction of protecting the C-7, 10 and attaching a side chain at C-13 position and subsequently deprotecting the group to form paclitaxel or docetaxel, and intermediates used therein.

The invention relates to a synthesizing method of a functionalized AuNc (gold nanocluster) based on BSA (bovine serum albumin) and application. The synthesizing method is characterized in that HAuCl4 is used as a precursor of Au (copper) atom, the BSA is used as a reductant and a protectant, and BSA-AuNCs is synthesized by a one-pot synthesis method. The synthesizing method has the beneficial effects that the synthesizing method is simple, and the reaction conditions are wild; the synthesized fluorescent AuNc has the advantages of good biocompatibility and photostability, good fluorescent characteristics, high yield of quantum, good water solubility, non toxicity, little inference by outside and the like; the synthesized BSA-AuNCs has higher selectivity on Cu<2+>, and can be applied to the quantitative detection and analysis of Cu<2+>; the detection method is simple and quick, the sensitivity is high, the toxicity is avoided, and the real-time qualitative and quantative detection of Cu<2+> is realized.

This invention relates to a method for preparing roinyl diterpene modified alpha-aminophosphate, and its anti-tumor application. The method comprises: reacting roinyl amine diterpenoid with substituted benzaldehyde and phosphite at a mol ratio of 1 :( 1-1.05) :( 1-1.1) by solvent synthesis, one-pot synthesis or solvent-free synthesis. The inroduction of roinyl diterpene into aminophosphate can largely improve the liposolubility and bioactivity of the compound. R1 structure comes from natural product rosin, thus has low toxicity.

The invention relates to a method for preparing Cu2O or CuO hollow submicron particles with controllable particle sizes by a water phase soft-template method, belonging to the technical field of the preparation of inorganic functional materials. In the invention, necklace-shaped soft matter clusters formed by sodium dodecyl sulfate and polyvinylpyrrolidone are taken as templates, cupric salt solution is added in soft clusters solution, after the pH value of the mixed solution is adjusted, hydrazine hydrate is taken as a reducing agent to quickly reduce copper ions by a one-pot method and assemble the copper ions into the Cu2O hollow submicron particles with controllable grain diameters and narrow particle size distribution; or further temperature programmed baking is carried out to oxidize the Cu2O hollow submicron particles to obtain CuO hollow submicron particles, the particle size and particle size distribution of which are similar to that of the Cu2O hollow submicron particles. The method of the invention has the advantages that: the products, Cu2O or CuO hollow submicron particles, have small particle sizes, narrow particle size distribution and good controllable property, the preparing technique is simple, the reaction at normal temperature and normal pressure is mild, the one-pot synthesis is easy to operate and repeat, and the method has low cost and is suitable for industrial production.

The invention relates to a process for the preparation of a quaternary ammonium hydroxide, in particular denatonium hydroxide, and the use thereof for the preparation of a quaternary ammonium salt, in particular of denatonium benzoate or a denatonium fatty acid derivative. Due to its extremely bitter taste, this latter compound is applied in the art as an aversive agent, biocide, antifoulant and flavorant. It is usually prepared from a quaternary ammonium halide in an organic environment, which after isolation and purification is converted to a hygroscopic and unstable hydroxide intermediate, which in turn is immediately converted to the salt of interest in the solvent in which it is prepared. It is now found that these isolation steps can be avoided by performing the reaction at aqueous conditions. This is more straightforwardly and does not require costly precautions to avoid contact while handling. Moreover, the process of the invention allows to produce the quaternary ammonium salt from a lignocaine compound in a one-pot synthesis involving mostly water.

The invention discloses a preparation method of branched polyethyleneimine and a shale intercalation inhibitor prepared from the branched polyethyleneimine. The branched polyethyleneimine is preparedby the following steps: S1. synthesizing aziridine; S2. with a polyamine compound and the aziridine as raw materials, preparing the branched polyethyleneimine by a stepwise synthesis process or a one-pot synthesis process, wherein the polyamine compound is polyethylene polyamine or alkylamine; the polyethylene polyamine is one of diethylenetriamine, triethylene tetramine, tetraethylenepentamine and pentaethylenehexamine; the alkylamine is one of ethylenediamine, propane diamine, butanediamine, pentamethylene diamine, nonamethylene diamine and decamethylene diamine. The shale intercalation inhibitor is prepared by proportionally mixing the branched polyethyleneimine with water. The branched polyethyleneimine synthesis method provided by the invention has the advantages of high yield and cheap raw materials and is suitable for large-scale industrial production; the shale intercalation inhibitor prepared from the branched polyethyleneimine can effectively alleviate the problem of unstableborehole wall caused by the hydration dispersion of shale.

A method of forming monodisperse metal chalcogenide nanocrystals without precursor injection, comprising the steps of: combining a metal source, a chalcogen oxide or a chalcogen oxide equivalent, and a fluid comprising a reducing agent in a reaction pot at a first temperature to form a liquid comprising assembly; increasing the temperature of the assembly to a sufficient-temperature to initiate nucleation to form a plurality of metal chalcogenide nanocrystals; and growing the plurality of metal chalcogenide nanocrystals without injection of either the metal source or the chalcogen oxide at a temperature equal to or greater than the sufficient-temperature, wherein crystal growth proceeds substantially without nucleation to form a plurality of monodisperse metal chalcogenide nanocrystals. Well controlled monodispersed CdSe nanocrystals of various sizes can be prepared by choice of the metal source and solvent system.

The invention relates to a three-component tandem synthesis method of a 2-cyano-3-arylpyrrole compound, wherein the reaction general formula is defined in the specification. According to the present invention, N,N-disubstituted formamide, trimethylsilyl cyanide and aryl olefin or aryl alkyne are subjected to one-pot synthesis under the actions of a Lewis acid catalyst and an oxidizing agent to prepare the 2-cyano-3-arylpyrrole compound; the used starting raw materials are simple; excluding the final product, the intermediates during the tandem conversion do not require separation and purification so as to reduce the coat input and the labor force input; and the simple and efficient preparation method is provided for the 2-cyano-3-arylpyrrole and the derivative thereof.

The invention belongs to the field of medicine and chemical engineering, and particularly discloses a preparation technology for 5-(2-cyano4-pyridyl)-3-(4-pyridyl)-1,2,4-troazole (topiroxostat). The preparation technology is characterized in that methyl isonicotinate serving as a compound II is used as a starting raw material, the compound II, phosphorus oxychloride, N,N-dimethyl formamide, iodine and 28% ammonium hydroxide form a compound III which is 2-cyano methyl isonicotinate in a one-pot synthesis mode, then a compound IV which is 2-cyano isonicotinyi hydrazine is formed through synthesis, a topiroxostat crude product Ia is prepared through condensing the compound IV which is 2-cyano isonicotinyi hydrazine and 4-cyanopyridine, salifying is performed on the crude product Ia and para-toluenesulfonic acid to form topiroxostat tosilate Ib, and finally the topiroxostat finished product I is obtained through desalting in a refined mode. The number of reactions steps is reduced, the yield of the finished product is increased, the reaction process is low in toxin and has small influences on environment, the reaction route is short, the cost is greatly lowered, the product purity is larger than 99.7%, the net contamination is smaller than 0.1%, and standard requirements are met.

The invention discloses a synthesis method for guanine, which includes the following steps: carrying out a cyclization reaction of guanidine nitrate and ethyl cyanoacrylate to obtain the compound of 2, 4-diamino-6-hydroxypyrimidine in formamide solvent, adding sodium nitrite, formamide and concentrated formic acid in turn, and carrying out nitrosation and reduction reaction with reducing agent and cyclization reaction to obtain the final product. The invention is the use of ''one-pot'', and the raw materials are fat chain ethyl cyanoacrylate and guanidine nitrate, which are directly from market, cheap and easy to get, without need of separation and purification of pyrimidine intermediates. Guanine is prepared by one step through effective control of reaction conditions, feeding sequence and ratio. The product is purified through adjusting pH, which has high yield and is easy to operate.

Ternary and quaternary Chalcopyrite CuInxGa1-xSySe2-y (CIGS, where 0≦x and y≦1) nanoparticles were synthesized from molecular single source precursors (SSPs) by a one-pot reaction in a high boiling solvent using salt(s) (i.e. NaCl as by-product) as heat transfer agent via conventional convective heating method. The nanoparticles sizes were 1.8 nm to 5.2 nm as reaction temperatures were varied from 150° C. to 190° C. with very high-yield. Tunable nanoparticle size is achieved through manipulation of reaction temperature, reaction time, and precursor concentrations. In addition, the method developed in this study was scalable to achieve ultra-large quantities production of tetragonal and quaternary Chalcopyrite CIGS nanoparticles.

The invention belongs to the field of electrochemical energy storage and discloses a spherical composite positive pole material for a lithium sulfur battery and a preparation method and application of the spherical composite positive pole material. The spherical composite positive pole material for the lithium sulfur battery is a porous carbon nanosphere / sulfur / polyaniline composite positive pole material and has a 'sandwich' spherical structure; according to a chemical coprecipitation method and a sulfur-bearing in-situ polymerization coated conductive polyaniline one-pot synthesis method, the porous carbon nanosphere / sulfur / polyaniline composite positive pole material is formed. The preparation method is simple in process and low in cost, and the consistency and stability of the product are high. The obtained composite positive pole material for the lithium sulfur battery is high in electronic and ionic conductivity, the sulfur bearing amount is high, diffusion of polysulfides is inhibited, and the composite positive pole material can be used for preparing a composite positive plate of the lithium battery. The obtained composite positive plate for the lithium sulfur battery is excellent in electrochemical performance, and is high in cycling stability and capacity retention ratio.

The present invention provides a synthetic method for an Apixaban drug intermediate. According to the invention, the reduction reaction of nitro groups in a compound 2 is conducted by sodium sulphide and amino groups in the compound 2 are protected by 5-chloro-pentanoyl. Therefore, the synthesis of Apixaban can be realized more simply and more directly. A novel one-pot synthesis method is provided by the invention and the method is mild in reaction conditions, high in safety coefficient, strong in maneuverability, simple in process and easy to industrialize. Meanwhile, a high-purity intermediate compound 14-1 can be obtained, so that the Apixaban of high purity and super-low impurity content can be obtained more easily. At the same time, the invention provides an effective and novel synthetic method for the preparation of an Apixaban key intermediate. By means of the method, the reaction efficiency is improved, and the production cost is lowered. The adoption of expensive reagents and severe reaction conditions can be avoided.

The invention relates to the synthesis of a 12-phenyl-benzo[b] xanthenetrione derivative, and especially relates to the synthesis of 3, 4-dihydro-12-phenyl-2H-benzo[b] xanthene -1, 6, 11 (12H)-trione, which is produced by subjecting the raw materials of aldehyde, 2-hydroxy-1, 4-naphthoquinone and an annular 1, 3-dicarbonyl compound to a one-step reaction by a three component one-pot synthesis method. With simple synthetic process and mild condition, the method of the invention has an overall yield over 80%.

A method of homogeneously forming metal chalcogenide nanocrystals includes the steps combining a metal source, a chalcogenide source, and at least one solvent at a first temperature to form a liquid comprising assembly, and heating the assembly at a sufficient temperature to initiate nucleation to form a plurality of metal chalcogenide nanocrystals. The plurality of metal chalcogenide nanocrystals are then grown without injection of either the metal source or the chalcogenide source at a temperature at least equal to the sufficient temperature, wherein growth proceeds substantially without nucleation to form a plurality of monodisperse metal chalcogenide nanocrystals. An optional nucleation initiator can help control the final size of the monodisperse crystals. Such synthesis, without the need for precursor injection, is suitable for the industrial preparation of high-quality nanocrystals.

Doping and functionalization could significantly assist in the improvement of the electrochemical properties of graphene derivatives. Herein, we report a one-pot synthesis of fluorinated graphene oxide (FGO) from graphite. The surface morphology, functionalities and composition of the resulting FGO have been studied using various surface characterization techniques, revealing that layer-structured nanosheets with ˜1.0 at. % F were formed. The carbon bound F exhibited semi-ionic bonding characteristic and significantly increased the capacitance of FGO compared to graphene oxide (GO). Further, the FGO has been employed for the simultaneous detection of heavy metal ions Cd2+, Pb2+, Cu2+ and Hg2+ using square wave anodic stripping voltammetry; and a substantial improvement in the electrochemical sensing performance is achieved in comparison with GO.

The invention relates to a one-pot synthesis super acid mesoporous material and preparation method, specifically involved a SO42- / ZrO2-SiO2 super acid mesoporous material and preparation method. Its characteristic lie in Zr(NO3)4 . 3H2O and CTAB were separately dissolved in ethanol solution, mix stirring, calculated as A; At the same time, the mixture of concentration 1mol / LH2SO4 and 2 mol / LHCl into Polyoxyethylene - polyoxypropylene - Polyoxyethylene triblock copolymer, and add to silicate lipid mixing make it uniform, calculated as B; put A into reaction kettle loaded with Teflon-lined, heating 3-4h under the 95-100degree centigrade, and after its removal, after cooling joined into B, the mixture evenly loaded into reaction kettle, at 95 ~ 100 degree centigrade crystallization 45 ~ 48 h, it would complete after washing filtrating roasting to remove template. The method prepared super acid mesoporous materials has short synthesis lead time, and have structured mesoporous structure, good thermal stability, and it demonstrated a positive catalytic activity in positive pentane isomerization reaction, it will become the important catalytic material of fine chemical,petrochemical and other aspects.

The invention belongs to the technical field of preparation of supported nano crystal catalysts and in particular relates to in situ controllable equipment for hydrotalcite-supported Pd nano crystal catalysts with different morphologies and research on activity of the hydrotalcite-supported Pd nano crystal catalysts in catalysis of a Heck coupled reaction. The synthesis process of the hydrotalcite-supported Pd nano crystal catalyst comprises the following step of: growing Pd nano crystals with different morphologies (cube, truncated octahedron and triangle) and different exposed crystal faces ({111} and {100}) in situ on the surface of hydrotalcite by adopting a one-pot synthesis method under the conditions of different reducing agents (polyvinylpyrrolidone and ethylene glycol) and surface capping agents (I<->, Cl<-> and polyvinylpyrrolidone) with a mixed solution composed of Na2PdCl4 and nitrate intercalation hydrotalcite. Besides, the synthesized hydrotalcite-supported Pd nano crystal catalysts with different morphologies are used for evaluating the Heck coupled reaction and researching a catalytic activity sequence of different exposed Pd crystal faces of the hydrotalcite-supported Pd nano crystal catalysts, and a foundation is laid for further reasonably designing an efficient supported nano crystal catalyst.

The invention relates to the field of environment-sensitive high polymer materials and aims to provide a method for realizing one-pot synthesis of pH and temperature double-sensitive ionic micro hydrogel. The method comprises the following steps: performing a free radical polymerization reaction on an N-alkyl acrylamide monomer, a double bond containing tertiary amine group, a polyhalogenated alkane compound and an initiator in an aqueous solution under oxygen-free conditions, dialyzing the obtained product for three days, performing ion exchange with organic cationic salt, and centrifuging to prepare the purified ionic micro hydrogel. The preparation method is simple and easily controllable, the obtained micro hydrogel has the pH and temperature double sensitivity, the excellent characteristics of the poly(ionic liquid) are introduced, and the micro hydrogel is high in purity, high in stability, high in swelling ratio and suitable for the fields of medicine controlled release and sensors and the like.

The invention discloses a one-pot synthesis method for 5-bromo-2-chloro-4'-ethoxy diphenylmethane. The method comprises the following continuous steps of: taking 2-chloro-5-bromobenzoic acid as a raw material, reacting it with thionyl chloride to generate 2-chloro-5-bromobenzoyl chloride, and adding an organic solvent, Lewis acid, phenetole and borohydride to undergo Friedel-Crafts acylation reaction and hydroboration reduction reaction so as to obtain the 5-bromo-2-chloro-4'-ethoxy diphenylmethane. The process involved in the invention has the advantages that the same Lewis acid is used as a catalyst in the Friedel-Crafts acylation reaction and the hydroboration reduction reaction, so that the catalyst consumption is greatly reduced, the operation is simple, and the intermediate needs no separation and purification. By effectively controlling the reaction conditions, and the charging sequence and proportion, the 5-bromo-2-chloro-4'-ethoxy diphenylmethane can be synthesized by one step, and fewer three wastes are discharged, the solvent recovery effect is good, and the production cost is low.