49results about How to "Synthetic method is convenient" patented technology

The invention relates to a method for synthesizing losartan and losartan intermediates and belongs to the technical field of medicine and medicine intermediates. 5-(4'-bromomethyl biphenyl-2-radical)-2-(1- methyl-1- phenylethyl) tetrazole and 2-butyl-4-chlorine-5-formyl radical imidazole are subjected to condensation, reduction and decomposition protection processes, and the losartan is obtained. The method has the advantages that the synthesis process is suitable for industrial production, in addition, the economic value can be generated, the synthesis process is safe, the raw material cost is saved, subsequent products are easy to treat, the reaction raw materials are single, and the synthesis method is convenient.

The invention relates to preparation of photocatalytic materials, and aims to provide a preparation method of a visible light response type MIL-100(Fe) photocatalytic composite material. The preparation method comprises the following steps: adding trimesic acid and sodium hydroxide in the same parts by mass into deionized water; conducting uniform mixing to obtain a trimesic acid / sodium hydroxidecomposite solution; dropwise adding the composite solution into an equal amount of ferrite solution, then adding a surfactant, and conducting uniform mixing and full reacting to form a turbid liquid;and filtering the turbid liquid, conducting washing, drying the obtained solid to obtain the MIL-100(Fe) photocatalytic composite material. The synthesis method at room temperature is more convenient,the crystallization is more stable, the application stability of the catalyst is greatly improved, and the recycling service life of the catalyst is greatly prolonged. The surfactant surface modification technique effectively reduces the grain size, greatly enhances the specific surface area of the material, and enhances the photocatalytic reaction efficiency. The utilization efficiency of the material on visible light can be remarkably improved, and relatively strong visible light catalytic activity is obtained.

The invention discloses a method for synthesizing citicoline and citicoline without using calcium phosphorylcholine chloride. Acylmorpholine is used as raw material, reacts with ethylene glycol to obtain ethylene glycol ester phosphoromorpholine, and then directly condenses with cytidylic acid to obtain ethylene glycol ester phosphoryl cytidylic acid, and finally tributylamine to ethylene glycol ester The ethylene glycol ester of phosphoromorpholine is ring-opened to give citicoline. There are three steps in the reaction, and the total yield is 78%. The method has cheap and easy-to-obtain raw materials, avoids the use of expensive and toxic DCC and calcium phosphorylcholine chloride, and the yield does not decrease significantly when the reaction scale is expanded to a scale of 500 g. The application of the present invention provides a new synthesis route for the synthesis of citicoline, and has potential application prospects.

The invention discloses a synthesis method of m-phenoxytoluene, relating to a synthesis method of a compound. The synthesis method comprises the following steps of: stirring and mixing m-chlorotoluene, sodium phenate, cuprous chloride, 8-oxyquinoline and polydiglycol in a reaction container at the room temperature, heating until the temperature of mixed liquor is 130-140 DEG C and then reacting for 8-9 hours under thermal-insulation stirring; finally, carrying out high-vacuum reduced pressure distillation and getting 100-110 DEG C of distillates to obtain the m-phenoxytoluene. In the invention, under the catalytic action of the cuprous chloride, the 8-oxyquinoline and the polydiglycol, the sodium phenate and the m-chlorotoluene are directly taken as raw materials to carry out single-step reaction to prepare the m-phenoxytoluene, wherein the m-chlorotoluene is a reactant and meanwhile takes the solvent action so that any solvent does not need to be additionally used, thereby greatly reducing cost.

The invention discloses a simple preparation method of a Z-type heterojunction composite material. Two semiconductors including Cu2O nanocrystals and g-C3N4 nanosheets are compounded to form a Z-type heterojunction, water is used as a proton source, efficient reduction of carbon dioxide into methanol is realized, and oxygen is generated at the same time. The synthesis method is simple, and water is used as a proton source without other sacrificial agents, so that the cost is effectively reduced, and good application prospects are achieved.

The invention discloses a method for synthesizing irbesartan and an intermediate thereof, and belongs to the technical field of preparation methods for medicines. The method comprises the following steps of: protecting 5-(4'-methylbiphenyl-2-yl)-2-(1-methyl-1-phenylethyl)tetrazole by using alpha-methyl styrene under the catalysis of organic acid through the novel convenient reaction process, brominating a benzyl group, condensing a solid phase and a liquid phase under phase transfer to obtain irbesartan protected by 1-methyl-1-phenylethyl, performing acid hydrolysis on the protection to obtain the irbesartan and 2-phenyl-2-propanol, and recovering the 2-phenyl-2-propanol to obtain the alpha-methyl styrene. The invention has the advantages that: the synthetic process is suitable for industrial production, economic value can be produced, the synthetic process is safe, the cost for raw materials is saved, the subsequent product can be easily treated, the reaction raw material is single, and the synthetic method is convenient.

The invention discloses a 2,6-dioxobicyclo[3.3.2]octane derivative and a synthesis method thereof. The synthesis method of the derivative is based on (E)-2-hydroxyl-1-naphthalene vinyl derivative The substrate is under the action of 1-chloromethyl-4-fluoro-1, 4-diazotized bicyclo[2.2.2]octane bis(tetrafluoroborate) salt and cuprous chloride, and the reaction obtains a novel 2,6-Dioxobicyclo[3.3.2]octane skeleton derivative compound. The method of the invention is simple to operate, and the reaction conditions are mild, and a novel 3D skeleton, two rings, three new chemical bonds (two C-O, one C-C) and four chiral centers are constructed in a one-pot reaction And a single stereo configuration was obtained, and a series of 2,6-dioxobicyclo[3.3.2]octane derivatives were constructed.

The invention discloses a bismuth sulfide / gadolinium oxide-entrapping ultrafine protein composite nanoparticle with a near-infrared photothermal effect and a multi-mode imaging function and a preparation method and application thereof. By formulation screening and process optimization, the bismuth sulfide / gadolinium oxide albumin ultrafine composite nanoparticle with the near-infrared photothermaleffect and the multi-mode imaging function is prepared in one step. The composite nanoparticle has good physicochemical stability, photostability, biocompatibility and tumor-targeting property, can remarkably enhance near-infrared fluorescence, photoacoustic, magnetic resonance, CT (computed tomography) and thermal signals at a tumor site, and realizes multi-mode-complemented tumor diagnosis, andmoreover, the composite nanoparticle can eliminate tumors under the excitation of near-infrared light; in particular, because the grain size of the nanoparticle is less than 5.5nm, the nanoparticle can be eliminated by the kidneys, and toxic and side effects are minor; a tumor can be diagnosed and treated at the same time, and the composite nanoparticle has a great potential in realizing accuratetumor diagnosis and treatment integration.

The invention relates to an organosilane ligand protected mixed valence ten-nuclear manganese cluster compound and a preparation method thereof. The preparation process comprises the following steps: dissolving alkali in an alcohol solvent, then adding trialkoxysilane containing a substituent group, carrying out reflux reaction, and carrying out prehydrolytic polycondensation to obtain a prepolymer; and then adding a metal salt solution of divalent manganese, transferring the mixture solution into a reaction kettle, heating, and carrying out solvothermal reaction to generate the organosilane protected mixed valence ten-nuclear manganese cluster compound. The invention also provides the mixed-valence ten-nuclear manganese cluster compound prepared by the method. The preparation method is realized through a solvothermal method, reaction conditions are easy to control, and the obtained manganese cluster compound is clear in structure and relatively high in purity, can be directly applied and has a huge application prospect.

The invention discloses an asymmetric synthesis method of chiral compounds derived from trans-tetrahydrofuran / pyranotetrahydroquinoline. The method uses 5-o-hydroxyphenyl-4-ene-1-pentanol derivatives and o- The aminobenzaldehyde derivative is reacted under the action of a chiral phosphoric acid catalyst to obtain a chiral compound derived from trans-tetrahydrofuran / pyranotetrahydroquinoline. The present invention provides an efficient, simple and convenient method for the first synthesis of trans-tetrahydrofuran / pyranotetrahydroquinoline derived chiral compounds by adopting dearomatization, Prins cyclization and aza-Michael addition series reaction modes resolve resolution. The method of the invention is simple to operate, and the reaction conditions are mild, and two new heterocycles, three new chemical bonds (C-O, C-C, C-N) and three adjacent quaternary carbon chirals are constructed in the one-pot reaction. A series of chiral compounds derived from trans-tetrahydrofuran / pyranotetrahydroquinoline were constructed.

The invention discloses a nano-cuprous oxide / silk fibroin complex and a preparation method thereof, which is characterized in that the main raw materials for preparing the complex include: 1.0-2.0 parts of silk fibroin, copper sulfate pentahydrate 0.5-2 parts, sodium hydroxide 0.58-1.92, vitamin C 0.7-2.8 parts. The preparation steps include: dissolving silk fibroin in deionized water to prepare a silk fibroin solution; preparing copper sulfate pentahydrate into a copper sulfate solution, adding it to the silk fibroin solution and stirring evenly, and then adding sodium hydroxide solution to adjust the pH value 10-12; vitamin C is formulated into a solution and added to the solution obtained in the above step (2), reacted at room temperature for 30-60 hours, dialyzed for 2-4 days, and freeze-dried to obtain nano-cuprous oxide / silk fibroin porous sponge. It can effectively hinder the agglomeration of nano-cuprous oxide particles, increase the stability of nano-cuprous oxide, prevent its oxidation, and prepare materials with various shapes.

The invention discloses a synthesis method of 4-allyl-3,5-disubstituted isoxazole, belonging to the technical field of organic synthesis. The synthesis method is as follows: in the reactor, add acetylene ketoxime ether substrate, 3-bromopropene, palladium catalyst, additive and solvent, stir and react at 70-80°C, and the reaction product is separated and purified to obtain 4-allyl -3,5-disubstituted isoxazoles. In the method of the present invention, a series of acetylenic ketone oxime ethers are obtained by reacting the product obtained through Sonogashira coupling of simple and easy-to-obtain acyl chlorides and alkynes with methoxyamine hydrochloride, the reaction conditions are mild, and there is no pollution to the environment. Potentially functional 4-allyl-3,5-disubstituted isoxazole compounds, the method is innovative and atom-economical, mild conditions, safe operation, and can be scaled up to 5 g scale without affecting the yield Therefore, it has potential practical value.

The invention discloses a polypyrrole / nickel hydroxide / foamed nickel integrated electrode and preparation method thereof. The polypyrrole / nickel hydroxide / foamed nickel integrated electrode is formed by loading foamed nickel with polypyrrole and nickel hydroxide, the total load amount of the polypyrrole and the nickel hydroxide on the foamed nickel is 0.9% to 1.4%, and the mass ratio of the polypyrrole to the nickel hydroxide is 1:3 to 2:1. An electrochemical test is performed on the integrated electrode, the electrode has excellent electrochemical performance, as the amount of polypyrrole increases, the specific capacitance of a material increases first and then decreases, and when the molar ratio of nickel nitrate to hexamine is 1:1 and the pyrrole monomer concentration is 0.05mol L<-1>, the specific capacitance of the electrode under the electric current density of 2A g<-1> reaches up to 2174F g<-1>, and the highest specific capacitance retention rate is achieved.

The invention discloses a boron-modified carbon nitride material as well as a preparation method and application thereof, urea and a boric acid solution are mixed and dissolved, a solvent is evaporated, recrystallization is performed, a recrystallized mixture is calcined, a B atom is enabled to enter a g-C3N4 skeleton by substituting a sp2-hybridized C atom in a 3-s-triazine ring, and the boron-modified carbon nitride material is prepared. The synthesis method is convenient, and the boron modified g-C3N4 photocatalyst material can be obtained through simple stirring, evaporation, grinding and air calcination in a muffle furnace. According to the preparation method, boric acid is utilized to enable B atoms to enter a g-C3N4 skeleton by replacing sp2-hybridized C atoms in a 3-s-triazine ring in a thermal polymerization process of urea, so that the g-C3N4 has higher photon-generated carrier separation capacity and reactive oxygen species generation capacity.

The invention belongs to the technical field of organic synthesizing and discloses a synthesizing method of a benzofuranone compound containing sulfonyl. The synthesizing method includes: adding substrate with the structure shown in formula 1, sodium sulfinate, silver salt catalyst, oxidizing agent and solvent into a reactor, performing stirring reaction under 80-90 DEG C, and separating and purifying reaction products to obtain the benzofuranone compound containing sulfonyl. The synthesizing method has the advantages that the sodium sulfinate which is simple and easy to obtain is used as the sulfonyl source, the cheap silver salt is used as the catalyst, the oxidizing agent is mild and free of environment pollution, and the functional benzofuranone compound containing sulfonyl is synthesized; the method has innovativeness and atom economy, is mild in condition and safe to operate and has potential practical value.