93 results about "Organic reaction" patented technology

The invention discloses a method for synthesizing deuterated olefin under catalysis of a palladium membrane by taking D2O as a deuterium source, and belongs to the technical field of synthesis of deuterated olefin building blocks. According to the method, a three-chamber electrolytic tank separated by a palladium membrane and an ion exchange membrane is used as a reactor, the palladium membrane is used as a working electrode, an electrolyte deuterium aqueous solution is used as an electrolyte, deuterium water is electrolyzed through a constant-potential electrolysis method, and formed active deuterium is transmitted to one side of an organic reaction taking absolute ethyl alcohol or cyclohexane as an organic solvent; and catalyzing an alkyne compound by using a palladium membrane modified by sodium thiophenol to perform reduction deuterization so as to synthesize a deuterated olefin compound with high selectivity, and further synthesizing a corresponding deuterated drug. The invention provides a green, efficient, high-universality and low-cost amplification synthesis method for synthesizing a deuterated olefin building block containing a functional group easy to reduce and hydrolyze, and the method has a wide application prospect.

The invention relates to the technical field of liquid chromatography, and discloses a mixed product liquid chromatography comprehensive analysis method which comprises the following steps: S1, mixing products: respectively mixing aldehyde compounds and ketone compounds with different mobile phases, and then injecting into an injection chromatographic system; s2, liquid chromatographic analysis: separating and analyzing a mixed product by using a liquid chromatograph; s3, performing qualitative analysis; on the basis of liquid chromatographic analysis, each peak in a chromatogram is identified. The method aims at qualitative and quantitative analysis of main substances (groups) in an organic reaction mixed product system; the method is suitable for analyzing the relative percentage content of products related to organic chemical reactions such as raw materials (nonylphenol) related to a core production process, nonylphenol formylation reaction, nonylphenol esterification reaction, phenolic ester Fris rearrangement reaction and the like, and samples in a refining process; the influence of absorption peaks and chromatographic line oscillation of other non-target substances on the content analysis result can be effectively avoided.

The invention relates to preparation of a crystalline allyl covalent organic framework material and application research of the crystalline allyl covalent organic framework material in benzamide cyclization green photocatalytic conversion. The SF-COF material is prepared by adopting a step-by-step synthesis method. The preparation method comprises the following steps: synthesizing a COF precursor by taking 1, 3-benzenetricarboxaldehyde and p-aminophenylacetonitrile as raw materials, and preparing the allylation covalent organic framework material with the electronic push-pull effect from the COF precursor and 5, 5 ', 5'-(benzene-1, 3, 5-triyl) tri (thiophene-2-formaldehyde) through a solvothermal method. The material is applied to the field of photocatalytic organic conversion, and benzamide cyclization and conversion of derivatives of benzamide are achieved under irradiation of a blue light LED. The prepared SF-COF has the advantages of efficient charge separation and electron conduction performance, good structural stability and chemical stability and the like. And a catalyzed organic reaction substrate has the advantages of wide universality range, good cycle stability and the like, and shows excellent photocatalytic conversion capability.

The invention provides a recombinant lipase mutant and application thereof in preparation of vitamin E succinate. The recombinant lipase mutant is obtained by performing single mutation on the 104th site, the 106th site, the 154th site, the 190th site, the 278th site, the 281th site or the 282th site of an amino acid sequence as shown in SEQ ID NO.1. The invention further provides a preparation method of the recombinant lipase mutant. The method has the beneficial effects that the recombinant lipase mutant for efficiently expressing the lipase CALB is used as a catalyst, so that the vitamin E succinate can be synthesized in an organic reaction system, the conversion rate of the vitamin E succinate can reach 90% or above, the relative enzyme activity of the recombinant lipase mutant is improved by 15% compared with that of a wild type, and the yield of the recombinant lipase mutant is improved. And the vitamin E succinate is synthesized by using the recombinant lipase mutant, so that the reaction condition is mild, the process operation is simple, the method is environment-friendly, the requirement on equipment is reduced, the production cost is greatly reduced, and the method has a wide application prospect in industrial application.

The invention relates to the field of photocatalytic organic reactions, in particular to a transition metal-based composite material for photocatalytic organic reactions and a preparation method of the transition metal-based composite material, and aims to solve the problems that an existing composite material based on transition metal functional groups is poor in light absorption effect and low in catalytic activity, and photocatalytic efficiency and photocatalytic stability are affected. And the wide application is limited. According to the preparation method, metalloporphyrin molecules with a high crosslinking degree are grafted on the surfaces of the carbon nanotubes, the number of active sites participating in a photocatalytic reaction is effectively increased, so that the photocatalytic activity is remarkably enhanced, and metalloporphyrin and the carbon nanotubes can exert unique advantages respectively and are matched with each other, so that the photocatalytic activity is improved. Through the synergistic effect of the two, photon energy can be more effectively absorbed, and generation and separation of photon-generated carriers are accelerated, so that the photocatalytic activity of the composite material is greatly improved, the efficiency and stability of a photocatalytic organic reaction can be remarkably improved, and the whole composite material is extremely excellent in the photocatalytic reaction.

The invention relates to the technical field of ionic liquid synthesis and catalytic synthesis of hydroxybutyl acrylate, in particular to a functional double-acid supported ionic liquid as well as a preparation method and application thereof. The functional double-acid supported ionic liquid comprises an MOFs (Metal-Organic Frameworks) material UiO-66-SO3H and a double-acid ionic liquid supported on the MOFs material. The synthesis of the double-acidified ionic liquid comprises the following steps: synthesizing a dimethyl monomer by adopting imidazole, pyrrolidine or morpholine; reacting the dimethyl monomer with 1, 4-butane sultone to generate sulfonic acid inner salt; and acidifying sulfonic acid internal hydrochloric acid. The functionalized double-acid supported ionic liquid has the advantages that the heat stability and the reusability are good; the product is immiscible with an organic reaction solvent and is easier to separate and recover; as a catalyst for catalyzing esterification reaction, the catalytic activity is obviously improved; as a solid catalyst in an esterification reaction, the catalyst can be applied to a fixed bed reactor, continuous esterification is realized, and the productivity is improved.

The invention provides a 1, 4-diaza-butanetriene compound as well as a synthesis method and application thereof, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: carrying out a first reaction on a compound 1 and a compound 2 in a solvent A, removing the solvent A after the reaction is finished, extracting with benzene or toluene, filtering, mixing with 12-crown ether-4, and stirring to obtain a compound 3; the synthesis method of the compound 3 provided by the invention is high in yield, simple to operate, mild in reaction, simple in required reaction condition control and high in speed. The obtained compound 3 has excellent stability and can be used for key intermediates in various organic reactions, such as preparation of alpha-diimine ligands.

The present application belongs to the technical field of heat dissipation devices, and particularly relates to a double-sided heat-conducting gasket with different properties and a preparation method thereof. The present application does not use the existing silica cloth as a reinforcing material, but uses a glass cloth blank without additional material and without a coating process as a medium for supporting two kinds of silica gel. The concentration of organic reactants and the molecular weight of silica gel on both sides of the glass cloth are calculated and controlled, and then the silica gel is subjected to stepwise calendering and vulcanization, so as to form a double-sided heat-conducting gasket with different properties on both sides, one side having adhesion and no air holes, and the other side having high strength and less oil bleeding. The present application firstly reduces the oil bleeding rate on the surface of the gasket with the traditional silica cloth as the reinforcing material, and secondly effectively reduces the dense air holes on the surface of the high-heat-conducting gasket with the additional reinforcing material below 0.5 mm, thereby enhancing the stability of the gasket performance.

The utility model relates to the technical field of reaction kettles, in particular to an organic reaction kettle and equipment, which comprises a kettle body, an upper cover and a clamping ring component, the upper cover is connected with the kettle body, the clamping ring component is respectively communicated with the kettle body and the upper cover, and at least three laser positioning components are uniformly distributed on the clamping ring component at intervals; therefore, by arranging the laser positioning assembly on the clamping ring component, the laser positioning assembly can calibrate the perpendicularity and parallelism between the kettle body and the upper cover in the process of covering the kettle body and the upper cover, so that the kettle body and the upper cover can be covered after being accurately aligned; the negative influence on the preparation of the anion exchange membrane or the damage to the reaction kettle caused by untight covering due to the fact that the kettle body and the upper cover do not forcibly cover the reaction kettle is avoided, and the production cost is greatly reduced.

The invention provides a 1, 4-dihydrobenzosilacyclohexane compound containing a polyfunctional group structure as well as a preparation method and application thereof, the preparation method specifically comprises the following steps: in the presence of a phosphine ligand, a palladium catalyst and a reaction medium, carrying out silicon-carbon bond activation and cycloaddition reaction on phenylpropargyl aldehyde and benzosilacyclobutane to prepare the 1, 4-dihydrobenzosilacyclohexane compound containing the polyfunctional group structure, and carrying out cycloaddition reaction on the 1, 4-dihydrobenzosilacyclohexane compound containing the polyfunctional group structure to obtain the 1, 4-dihydrobenzosilacyclohexane compound containing the polyfunctional group structure. The 2, 4-dihydrobenzo-silacyclohexane compound disclosed by the invention is applied to both material chemistry and medicinal chemistry. According to the present invention, the reaction condition is mild, the operation is simple, the substrate universality is strong, the crude product is subjected to rapid column chromatography impurity removal and vacuum concentration to obtain the pure product, the post-treatment is convenient, the finally obtained chemical selection is high, and the silicon-containing cyclohexane structure precursor can be widely used in various organic reactions and drug synthesis, and has considerable potential application value.

Process for producing alpha olefins comprising contacting ethylene, a zirconium based catalyst system comprising, a hydrocarbylmetal compound, a chain transfer agent, and optionally an organic reaction medium. Chain transfer agents which can be utilized include a) hydrogen, b) a compound comprising a hydrogen silicon bond, a compound having a hydrogen sulfur bond, a compound having a hydrogen phosphorus bond, or c) a transition metal compound chain transfer agent.

The present invention provides a D-D-π-A type organic photosensitizer and a synthesis method and application thereof, belonging to the field of photosensitizer and photodynamic therapy application of tumors. The present invention uses triphenylamine and carbazole as electron donors, malononitrile as an electron acceptor, and thiophene as an electron π bridge to synthesize an AIE type photosensitizer with mitochondrial targeting function through a series of simple organic reactions. The AIE type photosensitizer can be used in the synergistic photodynamic and ferroptosis treatment of tumors. The photosensitizer can realize tumor cell imaging and target mitochondria, and can selectively exert photodynamic and ferroptosis effects on tumor cells. It has good therapeutic effect and biosafety, and has strong application prospects in non-invasive tumor treatment.

The disclosure discloses a cyclodextrin glycosyltransferase with enhanced solvent tolerance and preparation thereof, belonging to the technical fields of enzyme engineering and genetic engineering. The disclosure constructs four cyclodextrin glycosyltransferase mutants with enhanced organic solvent tolerance. Among them, the mutant with the optimal tolerance to DMSO and methanol is G539I / R146F / D147N, which is 1.6 times and 1.7 times higher than that of WT, respectively; the mutant with the optimal tolerance to ethanol is R146F, which is 1.4 times higher than that of WT; the mutant with the optimal tolerance to acetone is G539I / R146F, which is 1.5 times higher than that of WT. The disclosure helps to expand the application of glycosyltransferases in organic reaction systems, improves the enzymatic efficiency of CGTase on natural hydrophobic substrates, and has great application prospects.

The invention relates to ylide-functionalized phosphane ligands, the production of same and use in transition metal compounds, as well as the use of same as catalysts in organic reactions.

The present invention provides a D-A type photochromic material and a preparation method thereof. The D-A type photochromic material uses compound 1 as the initial raw material, constructs a methyl-substituted spiropyran molecular skeleton SP-Br through two-step organic reactions, and then couples an aromatic conjugate unit to the spiropyran molecular skeleton through Suzuki coupling to obtain the product. The photochromic material and the preparation method thereof according to the present invention introduce an aromatic conjugate unit into the spiropyran molecular skeleton to construct a series of D-A type conjugate structures, effectively increasing the conjugate length of the molecule, regulating the HOMO / LUMO energy levels and band gap of the molecule, as well as the ring-opening / ring-closing rate of the molecule, thereby effectively regulating the photochromic ability and color change range of the material; the introduction of the conjugate unit can significantly increase the free volume of the material in the solid state, so that a series of D-A type conjugate materials can also produce an obvious photochromic process in the pure solid state.

The application discloses a metal nanocluster and a preparation method and application thereof, and provides a mixture comprising a reaction substrate, a metal salt, an alkali and a reducing agent, the metal salt and the reducing agent are reacted on site under the action of the alkali to prepare the metal nanocluster, and the metal nanocluster catalyzes a hydrogen functionalization reaction of the reaction substrate on site as a catalyst of an organic reaction. The metal nanocluster has the advantages of simple catalyst, low cost and high catalytic activity in catalyzing the hydrogen functionalization reaction of an unsaturated bond.

This invention provides a class of general-purpose chiral catalysts containing a cinchona primary amine arylformamide skeleton, along with their preparation methods and applications, belonging to the field of catalytic materials technology. The chiral catalysts provided by this invention link cinchona primary amine with oxazole / thiazole / imidazolium formamide structural units capable of coordination. Through the coordination of the oxazole / thiazole / imidazolium and amide coordinating groups with the central metal, they act as chiral ligands to catalyze a wider range of asymmetric reactions. They can also be used alone as chiral small-molecule catalysts for cinchona-like tertiary amine (thiourea) and square amides to catalyze asymmetric organic reactions. Furthermore, they can achieve synergistic (co-catalytic) catalysis of small molecules and metals in the same reaction system through different combinations. These chiral catalysts can be widely used as Lewis bases, Lewis acids, or small-molecule chiral catalysts and chiral ligands, possessing potential scientific and applied value in chiral sciences such as asymmetric catalysis, chiral synthesis, and chiral resolution.

There are many benefits to organometallic catalysis, especially in homogeneous catalysis for C(sp2)-H bond activation and new C-C bond formation reactions. These catalysts, which are mainly transition metal complexes with organic ligands, are very reactive and selective, which increases the range and effectiveness of different synthetic transformations. Their capacity to activate C-H bonds under mild reaction conditions is a key advantage as it allows for the direct C-H alkylation of aryl ketones without the need for transient functional groups. This reduces utilization of chemicals, cost and energy used in addition to streamlining synthetic routes. Furthermore, complex molecular architectures with high stereo- and regioselectivity may be formed with the help of organometallic homogenous catalysts, making precise synthesis of complex molecules possible. The present catalyst is easy to use, industrially scalable, recyclable, and provides excellent yields of C-H alkylated products from nonactivated alkyl halides. The reported methods need the use of excess (2-6 equivalent) of alkyl halides but this catalyst performs the catalytic reaction in the stoichiometric quantities of aryl ketone and alkyl halides.

A preparation method and use of a novel pure inorganic solid silicon-based sulfonic acid and / or phosphoric acid catalytic material are disclosed. The surface hydroxyl-rich metasilicic acid is used as the raw material, and by using a sulfonating reagent and / or phosphoric acid, the sulfonic acid group and / or the phosphoric acid group are bonded to the inorganic silicon material by chemical bonding to obtain a pure inorganic solid silicon-based sulfonic acid and / or phosphoric acid catalytic material. The catalytic material can be widely used in many acid-catalyzed organic reactions such as isomerization, esterification, alkylation, hydroamination of olefins, condensation, nitration, etherification, multi-component reactions and oxidation reactions. The inorganic solid silicon-based sulfonic acid and / or phosphoric acid catalytic material of the present invention has the advantages of high acid amount, high activity, good hydrothermal stability, no swelling, simple preparation, low cost, no pollution, no corrosion, easy separation and reusability.

The application discloses a kind of ultrafast metal-free and solvent-free preparation method for preparing symmetric and asymmetric disulfide, which comprises the following steps: at room temperature, raw material R-SH, R'-SH and oxidant and base are added to reaction bottle, shake rapidly for 10-30 seconds, and R-S-S-R' is prepared after the reaction product is purified;Wherein R in R-SH is aliphatic or aromatic group, R' in R'-SH is aliphatic or aromatic group;R in R-SH and R' in R'-SH are same or different;The aromatic group has substituent or no substituent, and the aliphatic is straight chain or has branch;The oxidant is chloroform, and the base is N, N-diisopropylethylamine (DIPEA).The method is simple in operation, high in yield (60-99%), ultrafast in reaction kinetics, greatly improves production efficiency, wide in applicability, avoids the use of organic reaction solvent, raw material is cheap and easy to obtain, and does not contain residual metal and other sticky contaminants from reagent and ligand, provides a safer and more effective method for the synthesis and production of symmetric and asymmetric disulfide-containing compounds.

The invention belongs to the technical field of electrocatalytic materials, and particularly relates to an electrocatalyst with a saturated coordination zinc diatom structure, a preparation method and application. Based on the principle that the boiling point of zinc chloride is lower than that of cadmium chloride and the boiling point of elemental cadmium is lower than that of elemental zinc, ZIF-8 serves as a precursor and is heated together with cadmium chloride, Zn in ZIF-8 can be volatilized at high temperature, Zn in ZIF-8 is replaced by cadmium chloride in the high-temperature process, cadmium (II) is reduced into elemental cadmium (Cd) steam by carbon generated by pyrolysis, and the elemental cadmium (Cd) steam leaves a reaction system; and finally, the catalyst (Zn DACs / N-C) with an excellent ORR performance and a zinc diatom structure is synthesized, and is expected to become a catalyst in fuel cell cathode reaction, automobile exhaust removal and organic reaction.

The invention discloses a mitochondrial targeting pyridinium cyanine photosensitizer compound, a preparation method, a compound and application thereof, and the pyridinium cyanine photosensitizer compound is generated through organic reaction by taking N-methyl-N-hydroxyethyl naphthylamine as an electron donor, pyridinium cyanine as an electron acceptor and double bonds as pi bridge connection. After the pyridycyanine photosensitizer compound is self-assembled and combined with HSA, specific fluorescent staining of mitochondria is achieved, active oxygen is efficiently generated under white light irradiation and directly acts on the mitochondria, and the cancer cell killing efficiency is improved. The preparation method is simple and efficient, and the prepared photosensitizer compound has a good photodynamic therapy effect and biological safety and has a good application prospect.

The invention relates to the field of organic synthesis, in particular to a post-treatment method for a catalytic hydrogenation reaction by using a copper-containing catalyst, which comprises the steps of adding an auxiliary agent and standing. According to the method, separation of the copper-containing catalyst and the organic reaction system is promoted in an efficient, economical, simple and convenient manner, on one hand, the purity and stability of catalytic hydrogenation products are improved, on the other hand, more copper-containing catalysts can be recycled, and generation of heavy metal waste is reduced.

Gold(I) complexes capable of absorbing light in the near-UV and / or visible region, and methods of making and using the same, are described. These gold(I) complexes have photochemical reactivity, such as strong absorption of near-UV and / or visible light, quenching rate constants of > 3.5 x 10 5 s ‑1 This enables them to catalyze photoredox reactions under near-UV and / or visible light, such as homocoupling of organic halides (e.g., alkyl halides and aryl halides), alkylation of 2-phenyl-1,2,3,4-tetrahydroisoquinolines, cyclization of indoles, reductive dehalogenation of aryl halides, and / or C-H bond cleavage, among others. The yields of products of photo-induced organic reactions catalyzed by the gold(I) complexes described herein can be higher than the yields of the same products formed from the same reactions under the same reaction conditions using [Au2(μ-dppm)2](Cl)2, [Ru(bpy)3](Cl)2, and / or [fac-Ir(ppy)3] at the same or higher loading than the loading of the one or more gold(I) complexes.

A cross-linked polystyrene-vinylpyridine copolymer, its preparation, and application in metal-catalyzed organic reactions. The copolymer is synthesized in a one-step process using styrene and 4-vinylpyridine as monomers, divinylbenzene as a cross-linking agent, potassium persulfate (K2S2O8) as an initiator, and water as a solvent. The copolymer is inexpensive and easy to prepare, and can quickly and effectively adsorb noble metal ions from complex solutions as a solid-phase adsorbent. Furthermore, the adsorbent can be desorbed by a solvent, and the noble metal-loaded adsorbent can also be directly used in organic catalytic reactions, achieving secondary utilization of the noble metal.

The invention discloses a method and device for preparing phenylhydroxylamine through electro-catalytic selective reduction of nitrobenzene, and the method comprises the following steps: carrying out a water oxidation reaction in an anode chamber of an electro-catalytic unit to generate oxygen and protons, and combining the protons with electrons and an oxidation-state electron carrier in a cathode chamber of the electro-catalytic unit to generate a reduction-state electron carrier; the electron carrier in the reduction state enters an organic reaction unit and is subjected to a reduction reaction with nitrobenzene, and an organic compound containing phenylhydroxylamine and an electron carrier in an oxidation state are obtained. The method is simple in system and gt in product selectivity; the conversion rate is gt; the product yield is generally higher than 95%. Compared with traditional industrial preparation of phenylhydroxylamine through catalytic hydrogenation, the method has the advantages that substances such as noble metal catalysts, organic solvents, sulfides and phosphides are not needed, the reaction cost is greatly reduced, and the steps of product separation are simplified.

The invention relates to a method for producing lithium alkylide compounds for use as anionic polymerization initiators and for various organic reactions. More specifically, the present invention relates to a process for preparing a lithium alkylide solution by reacting a lithium metal having a specific surface area of 1 to 100 cm2 / g with an alkyl halide in an organic solvent medium under high turbulence conditions wherein the molar ratio of lithium metal to alkyl halide is 2.5: 1 to 5.5: 1. The technical result achieved by the invention is that a high lithium alkylide yield is achieved using a lithium metal having a low specific surface area under high turbulence conditions and at a molar ratio of lithium metal to alkyl halide of 2.5: 1 to 5.5: 1, comparable to the lithium alkylide yield achieved using finely dispersed lithium metal particles having a high specific surface area.

The invention relates to a method for carrying out redox reactions with a three-phase electrode, having two separate phases, comprising an organic phase containing an amphiphilic organic reactant and / or an electrochemically inert organic solvent and an aqueous phase containing a hydrophilic reactant and / or an aqueous solvent with a hydrophilic reactant, wherein the organic and the aqueous phase are separated from one another by a permeable membrane.

The present invention discloses a 3-indole-deoxycarbon glycoside and a preparation method thereof. The present invention uses an easily synthesized olefin sugar donor and an indole derivative as raw materials, and catalyzes the indole C-3 glycosylation reaction with an inexpensive metal catalyst to construct the 3-indole-deoxycarbon glycoside. The preparation method can prepare the 3-indole-deoxycarbon glycoside with high regioselectivity and stereoselectivity. The preparation method of the present invention has the advantages of readily available raw materials, mild reaction conditions, wide substrate applicability, and simple operation. The prepared 3-indole-deoxycarbon glycoside has potential biological activity and can be widely used as a fine chemical intermediate in various organic reactions and the synthesis of drugs for the treatment of type 2 diabetes, and has considerable application value.

The present invention provides an application of immobilized phospholipase A1 in the preparation of phosphatidyl DHA. The specific process is as follows: cobalt nitrate hexahydrate and 2-methylimidazole are respectively dissolved in anhydrous methanol to obtain a cobalt nitrate hexahydrate solution and a 2-methylimidazole solution. The 2-methylimidazole solution is added dropwise to the cobalt nitrate hexahydrate solution, stirred and reacted, allowed to stand, and dried to obtain ZIF-67 nanomaterials. The ZIF-67 nanomaterials are suspended in a sodium phosphate buffer solution, a phospholipase A1 solution is added, the pH is adjusted, and the mixture is incubated on a shaker, centrifuged and dried to obtain ZIF-67 nanomaterial-immobilized phospholipase A1. A substrate composed of free fatty acids and soybean lecithin and the immobilized phospholipase A1 are subjected to a catalytic reaction in an organic reaction system, and phosphatidyl DHA is obtained by separation and purification. The immobilized phospholipase A1 has good stability, catalyzes the preparation of phosphatidyl DHA, and the DHA incorporation rate is as high as 51.04%.