44results about How to "Gentle synthesis method" patented technology

The invention provides sulfamate serving as an indoleamine-2, 3-dioxygenase inhibitor and a preparation method and application thereof. The structure of the inhibitor is shown in the general formula I, wherein definitions of X, R1, R2, R3, R4, R5 and n are shown in the description and the claim. The invention further discloses the preparation method of the inhibitor. The compound shown in the general formula I can serve as the indoleamine-2, 3-dioxygenase inhibitor and is used for preparing medicine for preventing and / or treating indoleamine-2, 3-dioxygenase mediated diseases. The general formula I is shown in the description.

The invention relates to a fasudil hydrochloride compound and a novel method thereof. The method comprises the following steps of: in the presence of a solvent, performing sulfonation reaction on a chlorosulfonic acid serving as a sulfonating agent and isoquinoline to generate a 5-isoquinolinesulfonic acid; reacting the 5-isoquinolinesulfonic acid with thionyl chloride under a heating condition to generate isoquinoline-5-sulfonyl chloride hydrochloride; and dissolving the isoquinoline-5-sulfonyl chloride hydrochloride with ice water, adjusting the pH value of the solution with sodium bicarbonate, reacting the solution with homopiperazine, adjusting the pH value again with a hydrochloric acid, and concentrating under reduced pressure and recrystallizing to prepare the fasudil hydrochloride compound. The synthesis method of the invention has the advantages of mild reaction conditions, high yield and easy industrial production.

The invention belongs to the field of polymer materials, relating to a method for synthesizing acetoacetate ester modified polymer. The method comprises the following steps: taking polymer containing hydroxyl and micromolecule acetoacetate ester as raw materials, and performing reaction under the condition of microwave irradiation; and the equation is shown in the specification, wherein R2(OH)n is polymer containing multi-hydroxy. The invention synthesizes the polymer of which side chains or chain ends have a plurality of acetoacetate ester groups by the process of catalytic ester exchange. The synthetic method has the advantages of high efficiency, mild synthetic method and high safety. In addition, in the method, the catalyst can be added, thereby improving synthetic efficiency; the synthetic rate of the method is greatly improved compared with the prior art; and the reaction time is shortened to 2-30min.

The invention relates to a gold-sliver alloy two-dimensional ordered nano film prepared by in-situ interface transformation and a method for preparing the gold-sliver alloy two-dimensional ordered nano film. The method adopting a two-step transformation process comprises the following steps: by taking a single-layer polystyrene sphere self-assembled film as a template, preparing a polystyrene-silver nano net film with a controllable thickness by a gas slow release method; transferring the polystyrene-silver nano net film to a solution surface of a chloroauric acid and disodium hydrogen phosphate solution, and obtaining the gold-sliver alloy two-dimensional ordered nano film by carrying out in-situ replacement reaction; and finally, soaking the gold-sliver alloy two-dimensional ordered nano film to remove the polystyrene template. The synthetic method has the advantages of being simple, quick, gentle and low in energy consumption, and meets the requirements of green chemistry; the smallest constitutional unit of the prepared gold-sliver alloy two-dimensional ordered nano net film is a hollow gold-sliver alloy nano particle; and the film has the advantages of being great in specific surface area, good in permeability, low in density and the like, can be loaded on substrates of different types, has the advantages of being convenient to recycle, and easy to enlarge a product, and can be widely applied to the fields of photoelectrocatalysis, biosensing, biological medicine carrying and the like.

The invention discloses an indoleamine-2,3-dioxygenase inhibitor containing sulfoximine subjected to nitrogen alkylation and arylation and a preparation method thereof. The inhibitor disclosed by the invention has a structure shown in a general formula (I), wherein the definitions of X, R1, R2, R3, R4, R7, R8, R9, n and m are shown in a description and claims. The invention also discloses a preparation method of the inhibitor. According to the indoleamine-2,3-dioxygenase inhibitor disclosed by the invention, a compound shown in the general formula (I) can be used as the indoleamine-2,3-dioxygenase inhibitor and can be used for preparing medicines for preventing and / or treating indoleamine-2,3-dioxygenase-mediated diseases. The formula (1) is shown in the description.

The invention relates to an aptamer modified triazine covalent organic framework composite material and a preparation method and application thereof. The aptamer modified triazine covalent organic framework composite material disclosed by the invention comprises a triazine covalent organic framework, gold nanoparticles and an aptamer, wherein the gold nanoparticles are supported on the triazine covalent organic framework; and the aptamer is bonded onto the surface of the gold nanoparticles. When the sequence of the aptamer is 5'-SH-(CH2)6-(ACAG4TGTG4)2-3', the composite material disclosed by the invention can be applied to enrichment of insulin in biological samples. The aptamer modified triazine covalent organic framework composite material disclosed by the invention combines the advantages of the covalent organic framework such as large specific surface area and multiple adsorbable sites and the advantage of the aptamer such as specific recognition, has excellent selectivity, and canprovide an economic, high-efficiency and high-sensitivity biological analysis method.

The invention discloses a platinum complex for inhibiting cell SKOV3 and a synthesis method of the platinum complex, belongs to the technical field of medicines, and aims to provide a cell SKOV3 inhibiting platinum complex synthesized from rutaecarpine as structural basis and DMSO as an auxiliary ligand. The invention further provides a synthesis method of the platinum complex. The structural formula of the platinum complex is as shown in the description. The platinum complex can be used for preparing anti-tumor drugs.

The invention relates to targeted nanometer photosensitizer for photodynamics deep tumor therapy and a preparing method thereof. According to the preparing method, protein, or polypeptide or amino acid is used for reacting with a soluble copper salt solution, and the monovalence protein chelated targeted nanometer photosensitizer or the polypeptide-copper chelated targeted nanometer photosensitizer or the amino acid-copper chelated targeted nanometer photosensitizer is obtained after reduction. Under excitation of X rays with the dosage much lower than a general radiotherapy dosage, the targeted nanometer photosensitizer can generate strong fluorescence and has a photodynamics therapy effect on tumors. The targeted nanometer photosensitizer is small in particle size, good in water solubility, small in toxic and side effect and capable of being endocytosed by deep tumor cells easily. The X rays serve as an excitation light source of the targeted nanometer photosensitizer, the therapy efficiency is high, and the problems that existing photodynamics therapy cannot be carried out on the deep tumors, and skin phototoxicity is caused can be solved. Reaction conditions of the photosensitizer are moderate, and the photosensitizer can be industrially manufactured, achieves energy conservation and environment protection, can promote the silkworm breeding and mulberry growing industrial chain to develop in the high value-added industry direction, and has good economic benefits, social benefits and ecological benefits.

The invention provides a preparation method of a phosphate ester or a phosphite ester. The preparation method comprises the following step: reacting an inorganic phosphate or an inorganic phosphite with a silicon-substituted cycl-lactam compound shown in a formula 3) to obtain the phosphate ester shown in a formula 1) or the phosphite ester shown in a formula 2). The preparation method provided bythe invention not only can be used for preparing phosphate esters, but also can be used for preparing phosphite esters. The synthetic method disclosed by the invention is mild and stable in reaction,convenient to operate, high in yield, high in purity and low in energy consumption in the reaction process, and is a universal synthetic method for synthesizing phosphate esters or phosphite esters.

The invention discloses a tryptanthrin-platinum complex, and a synthesis method and an application thereof, and belongs to the technical field of medicines, and aims at providing a tryptanthrin-platinum complex, a synthesis method thereof, and a new use of the tryptanthrin-platinum complex in the antitumor field. The structural formula of the tryptanthrin-platinum complex is shown in the description, and the tryptanthrin-platinum complex is used for preparing antitumor medicines.

The invention belongs to the field of pharmaceutical chemistry and relates to a novel phosphoinositide 3-kinase inhibitor, a preparation method and an application thereof. Specifically, the present invention provides a compound having the structure of formula I, which can be used as an efficient PI3K inhibitor and has various pharmacological activities such as tumor resistance, resistance to neurodegenerative diseases (such as Alzheimer's disease), inflammatory resistance, etc.

The invention relates to a carbon felt-loaded cerium-doped alpha-FeOOH nanosheet array electrode, a preparation method thereof and application of the carbon felt-loaded cerium-doped alpha-FeOOH nanosheet array electrode in electro-Fenton water treatment. The preparation method comprises the following steps: firstly, preparing an aqueous solution containing an iron source and a cerium source; and adding glycerol and a conductive carbon felt, carrying out hydrothermal reaction, and carrying out post-treatment to obtain the nanosheet array electrode. The nanosheet array electrode can be used as a cathode material for removing organic pollutants through electro-Fenton reaction. Compared with the prior art, the cerium-doped alpha-FeOOH nanosheet array loaded carbon felt electrode prepared by the preparation method disclosed by the invention is simple in synthesis method, free of metal dissolution, stable in reutilization performance and high in mineralization rate, and has a wide prospect in industrial wastewater treatment.

The present invention discloses an efficient IDO / TDO double inhibitor containing a nitrogen heterocyclic helix structure, and in particular, relates to a compound of formula (I) or pharmaceutically acceptable salt, stereoisomers, or tautomers, or prodrugs thereof. The compound of the formula (I) can be used as an indoleamine-2,3-dioxygenase inhibitor and tryptophan-2,3-dioxygenase for preparationof drugs for prevention and / or treatment of indoleamine-2,3-dioxygenase and tryptophan-2,3-dioxygenase-mediated diseases.

The invention specifically relates to a biological preparation method for a photoelectric conversion material, belonging to the field of photoelectrochemistry. The biological preparation method comprises the following steps: with sulfate-reducing bacteria used as a biological material, carrying out enrichment culture in a culture solution, then adding an excess aqueous CdSO4 solution, carrying out a reaction for 30-60 minutes at room temperature, and then carrying out centrifugation and drying so as to obtain the biosynthetic photoelectric conversion material. The preparation method of the invention is simple in process, easy to operate and low in cost, and has potential application value in the research fields of photoelectrochemical solar cells, photoelectrochemical decomposition of water, photoelectrochemical analysis, etc.

A targeted nano-photosensitizer for photodynamic therapy of deep tumors and its preparation method, using protein, polypeptide or amino acid to react with a soluble copper salt solution, and then reducing to obtain a monovalent protein chelated targeted nano-photosensitizer, polypeptide copper chelated Or amino acid copper chelation targeted nano photosensitizer. The targeted nano-photosensitizer can generate strong fluorescence under X-ray excitation far lower than the dose of ordinary radiotherapy, and has photodynamic therapy effect on tumors. The targeted nano-photosensitizer has small particle size, good water solubility, low toxic and side effects, and is easily endocytosed by deep tumor cells. At the same time, the excitation light source of the targeted nano-photosensitizer is X-rays, which has high treatment efficiency and can solve the problems that existing photodynamic therapy cannot perform photodynamic therapy on deep tumors and skin phototoxicity. The photosensitizer has mild reaction conditions, can be manufactured industrially, is energy-saving and environment-friendly, can promote the development of sericulture industry chains towards high value-added industries, and has good economic, social and ecological benefits.

Disclosed in the present invention are an indoleamine-2,3-dioxygenase inhibitor and a preparation method therefor. The structure of the inhibitor of the present invention is shown in general formula (I), wherein the definitions of X, R1, R2, R3, R4, R7, R8, R9, n and m are as shown in the description and the claims. Also disclosed in the present invention is a preparation method for the inhibitor. The compound in general formula (I) of the present invention can be used as an indoleamine-2,3-dioxygenase inhibitor for the preparation of a drug for preventing and / or treating diseases mediated by indoleamine-2,3-dioxygenase.

The invention discloses a Fe<3+> detection hyperbranched conjugated polymer and a preparation method and application thereof. A structural unit of the polymer is as shown in the specification, wherein R refers to one of carbomethoxy, carbethoxy, tert-butoxycarbonyl, cyano, nitro and -COONa arbitrarily. By MBH-type reaction synthesis, mild reaction conditions, environment friendliness and freeness of metal catalyst residues are realized; since Fe<3+> ions have an evident quenching effect on fluorescence of a tetrahydrofuran solution or an aqueous solution of the synthesized hyperbranched conjugated polymer, the hyperbranched conjugated polymer can be used for detection of Fe<3+> ions in an aqueous phase or an organic phase and is high in Fe<3+> ion selectivity and low in Fe<3+> ion detection limit.

The invention discloses a water-soluble multifunctional group oligomeric silsesquioxane and a synthetic method of the water-soluble multifunctional group oligomeric silsesquioxane. The synthetic method comprises the steps that: 1) 1 mol of octavinyl oligomeric silsesquioxane, 0.1 to 10 mol of dry first solvents, 8.1 to 20 mol of compounds containing sulfydryl and dimethylamino and 0.005 to 0.1 mol of free radicals light initiators are sequentially added into a reactor, the light irradiation reaction is carried out for 1 to 24 hours at 0 to 40 DEG C, reduction vaporization is carried out for removing the first solvents to obtain intermediates; and 2) 0.1 to 10 mol of dry second solvents are added, 8.1 to 20 mol of compounds containing active halogen substituents are dripped at 20 DEG below zero to 0 DEG C, after 0.1 to 48 hours, 1 to 100 mol of low-polarity solvents are added, obtained sediments are separated and dried, and target products are obtained. The water-soluble multifunctional group oligomeric silsesquioxane can be used for biological materials, paint components and nanometer structure units.

The invention relates to a preparation method of a CDKs inhibitor of a beta-carboline parent nucleus and an anti-tumor application of the CDKs inhibitor, and particularly provides a novel beta-carboline derivative with CDKs inhibition activity, an application of the novel beta-carboline derivative in anti-tumor, and a preparation method of the compound. The synthesis method is simple and mild; the compound disclosed by the invention can effectively inhibit CDK4, and has the activities of resisting tumor cell proliferation activity, inhibiting tumor cell migration and invasion, inducing tumor cell apoptosis, inhibiting nude mouse subcutaneous tumor-bearing growth and the like. Therefore, the compound as a lead compound plays an important role in tumor treatment.

The invention belongs to the technical field of SAPO-11 molecular sieves, and discloses a normal-pressure synthesis method of an SAPO-11 molecular sieve. The method comprises the following steps: sequentially adding water, an aluminum source, a phosphorus source, organic amine, a silicon source and a carbon material into a container according to a specific molar ratio, performing stirring to prepare sol, and heating and crystallizing the sol under a microwave condition to obtain a molecular sieve SAPO-11, wherein the molar ratio of the water to the aluminum source (in terms of Al2O3) to the phosphorus source (in terms of P2O5) to the organic amine to the silicon source (in terms of SiO2) to the carbon material is (60-120):1.0:1.0:(1.1-1.4):(0.2-1.0):(0.01-0.50). The method has the advantages of mild conditions, smooth synthesis of the molecular sieve SAPO-11, substantial shortening of the synthesis induction period of the molecular sieve, and effective inhibition of the aggregation phenomenon of small crystal grains.

The invention relates to a fasudil hydrochloride compound and a novel method thereof. The method comprises the following steps of: in the presence of a solvent, performing sulfonation reaction on a chlorosulfonic acid serving as a sulfonating agent and isoquinoline to generate a 5-isoquinolinesulfonic acid; reacting the 5-isoquinolinesulfonic acid with thionyl chloride under a heating condition to generate isoquinoline-5-sulfonyl chloride hydrochloride; and dissolving the isoquinoline-5-sulfonyl chloride hydrochloride with ice water, adjusting the pH value of the solution with sodium bicarbonate, reacting the solution with homopiperazine, adjusting the pH value again with a hydrochloric acid, and concentrating under reduced pressure and recrystallizing to prepare the fasudil hydrochloridecompound. The synthesis method of the invention has the advantages of mild reaction conditions, high yield and easy industrial production.

The invention relates to a preparation method of a hierarchical porous metal organic framework chiral sensing probe, which comprises the following steps of providing a hierarchical porous metal organic framework microsphere with a regular pore structure, fixing amino acid oxidase on the hierarchical porous metal organic framework microspheres to obtain hierarchical porous metal organic framework microspheres fixed with enzymes, and loading the amino acid oxidase in pore channels of the hierarchical porous metal organic framework microspheres through adsorption, fixing fluorescent molecules on the hierarchical porous metal organic framework microspheres fixed with enzyme to obtain the hierarchical porous metal organic framework chiral sensing probe, and loading the fluorescent molecules in pore channels of the hierarchical porous metal organic framework microspheres through adsorption. The invention also provides the hierarchical porous metal organic framework chiral sensing probe obtained by the preparation method and application thereof. By fixing different amino acid oxidase as a chiral recognition center, the amino acid can be recognized and the content of the amino acid can be analyzed in a high-sensitivity and high-specificity manner.

The invention relates to the field of chiral organosilanes, and specifically discloses a bichiral central cyclopropylsilane compound shown in formula (I) and a preparation method thereof, comprising: combining cyclopropene shown in formula (II) with diphenyl Cyclopropylsilane compounds with high yield and high enantioselectivity were efficiently synthesized by asymmetric hydrosilylation reaction of cyclopropylsilane. Compared with the traditional [2+1] cycloaddition and 1,3-cyclization substituted cyclopropylamino reactions, it is a more direct and effective method for the synthesis of cycloalkane compounds, and can obtain a variety of different compounds that cannot be prepared by traditional methods. Cyclopropylsilane compounds with substituents are widely used in the fields of materials chemistry and medicinal chemistry.

The invention discloses a synthesis method of a cabozantinib dimer. The method comprises the following steps: preparation of 4-chloro-6,7-dimethoxyquinoline, preparation of an intermediate 1, and preparation of a cabozantinib dimer impurity; and preparation of cabozantinib dimer impurities: adding an organic solvent into a reactor at room temperature, stirring for 10 min, adding cyclopropanedicarboxylic acid, stirring for 20 min, then adding an intermediate 1 with the mass ratio of the intermediate 1 to the cyclopropanedicarboxylic acid being 400:115, carrying out a reaction for 3 h, enablingthe raw material to remain 4%, heating to 45 DEG C until the reaction is complete, adding water, separating out the product, and carrying out suction filtration to obtain the cabozantinib dimer impurities. By adopting the synthesis method of the cabozantinib dimer, no high-temperature and high-pressure reaction exists in the synthesis process, the synthesis method is mild and easy to operate, allthe steps are mild and controllable, the operation is simple, and the controllability is high.

The invention discloses a rutaecarpine alkali gold salt as well as a synthesis method and an application thereof, belongs to the technical field of medicines and aims to provide the rutaecarpine alkali gold salt, the synthesis method thereof and the novel application of the rutaecarpine alkali gold salt in the antitumor field. The structural formula of the rutaecarpine alkali gold salt is as shown in the description. The rutaecarpine alkali gold salt can be used for preparing an antitumor medicine.

The invention relates to an alpha-pyrone compound and a synthesis method thereof. According to the novel method for efficiently synthesizing the alpha-pyrone compound, bromoacetophenone and cyclopropenone are catalyzed by DMAP to be subjected to a [3 + 3] cyclization reaction under the alkaline heating condition to generate the alpha-pyrone compound. The method is easy to operate and easily available in raw materials, and has potential economic benefits. Because the alpha-pyrone medicine is widely applied clinically, the provided new method for synthesizing the alpha-pyrone compound and is expected to provide a new direction for clinical application of pyrone. The synthesis method disclosed by the invention has the advantages of simple operation, easily available raw materials, mild reaction conditions, no need of a metal catalyst and easy separation and purification of the product, solves the technical difficulties of complex steps and complex raw materials of the synthesis method in the prior art, is a breakthrough of the existing synthesis technology, and has a very high application value.

The invention relates to alpha-TeO2 of a micro structure, which is of an alpha-TeO2 material with the thickness of 0.5 to 1 micrometer, the width of 3 to 5 micrometer and close-packed small wafers. The alpha-TeO2 is made by adopting Beta-TeO2 as the raw material to be hydrothermal treated in the water solution of NaOH and NH4NO3. The alpha-TeO2 of the micro structure can be used as an excellent tellurium-source to prepare combined metal oxide catalyst. The invention discloses a production method of alpha-TeO2.

The invention relates to an aptamer-modified triazine covalent organic framework composite material and its preparation method and application. The aptamer-modified triazine covalent organic framework composite material of the present invention includes a triazine covalent organic framework, gold nanoparticles and aptamers, and the gold nanoparticles are immobilized on the triazine covalent organic framework On, the aptamer is bound to the surface of the gold nanoparticle. When the sequence of the aptamer is 5′‑SH‑(CH 2 ) 6 ‑(ACAG4TGTG4) 2 -3', the composite material of the present invention can be applied to the enrichment of insulin in biological samples. The aptamer-modified triazine covalent organic framework composite material of the present invention combines the advantages of large specific surface area of ​​covalent organic framework, many adsorption sites and specific recognition of aptamers, has good selectivity, and can Provide an economical, efficient, and highly sensitive bioanalytical method.