282results about "Hydrazone preparation" patented technology

One aspect of the present invention relates to ligands for transition metals. A second aspect of the present invention relates to the use of catalysts comprising these ligands in transition metal-catalyzed carbon-heteroatom and carbon-carbon bond-forming reactions. The subject methods provide improvements in many features of the transition metal-catalyzed reactions, including the range of suitable substrates, reaction conditions, and efficiency.

A polymerizable compound has a practical low melting point, excellent solubility in a general-purpose solvent, and can produce an optical film at low cost, exhibits low reflected luminance, and achieves uniform conversion of polarized light over a wide wavelength band, an optically anisotropic article. A carbonyl compound is useful as a raw material for producing the polymerizable compound. (In the formula (I), Y1 to Y8 represent —C(═O)—O—, G1 and G2 represent a C1-20 divalent linear aliphatic group, Z1 and Z2 represent a C2-10 alkenyl group that is unsubstituted, or substituted with a halogen atom, Ax represents a C2-30 organic group with at least one aromatic ring, Ay represents a hydrogen atom or C1-20 alkyl group, A1 represents a trivalent aromatic group, A2 and A3 represent a C3-30 divalent alicyclic hydrocarbon group, A4 and A5 represent a C6-30 divalent aromatic group or the like, and Q1 represents a hydrogen atom.)

One aspect of the present invention relates to novel ligands for transition metals. A second aspect of the present invention relates to the use of catalysts comprising these ligands in transition metal-catalyzed carbon-heteroatom and carbon-carbon bond-forming reactions. The subject methods provide improvements in many features of the transition metal-catalyzed reactions, including the range of suitable substrates, reaction conditions, and efficiency.

The present invention relates to copper-catalyzed carbon-heteroatom and carbon-carbon bond-forming methods. In certain embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-nitrogen bond between the nitrogen atom of an amide or amine moiety and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. In additional embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-nitrogen bond between a nitrogen atom of an acyl hydrazine and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. In other embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-nitrogen bond between the nitrogen atom of a nitrogen-containing heteroaromatic, e.g., indole, pyrazole, and indazole, and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. In certain embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-oxygen bond between the oxygen atom of an alcohol and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. The present invention also relates to copper-catalyzed methods of forming a carbon-carbon bond between a reactant comprising a nucleophilic carbon atom, e.g., an enolate or malonate anion, and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. Importantly, all the methods of the present invention are relatively inexpensive to practice due to the low cost of the copper comprised by the catalysts.

The invention provides dihydric alcohol containing an acylhydrazone bond, dihydric alcohol containing an acylhydrazone bond and a disulfide bond, a self-repairing polyurethane elastomer and a preparation method thereof. The polyurethane elastomer is prepared from the dihydric alcohol containing the acylhydrazone bond or the dihydric alcohol containing the acylhydrazone bond and the disulfide bond and a polyurethane prepolymer. The dihydric alcohol containing the acylhydrazone bond is prepared from a dihydrazide monomer and hydroxy aldehyde. The dihydric alcohol containing the acylhydrazone bond and the disulfide bond is prepared from a dithio lipid monomer, hydrazine hydrate and hydroxy aldehyde. The polyurethane prepolymer is prepared from a polyester or polyether polyol monomer and diisocyanate. After the self-repairing polyurethane elastomer is mechanically damaged, the acylhydrazone bond or the disulfide bond on a crosslinked polymer molecular chain achieves material self-repairing through dynamic exchange reaction. The self-repairing crosslinked polyurethane elastomer material is simple in preparation, can achieve self repairing at room temperature, is high in repairing capability, short in repairing time and capable achieving many times of self repairing and has better mechanical properties.

The present invention provides transition-metal-catalyst-based methods for the arylation and vinylation of activated methyl, methylene, and methine carbons with aryl halides, vinyl halides, and the like. The methods of the invention provide several improvements over existing methods, including the ability to synthesize efficiently and under mild conditions α-aryl and α-vinyl products from a wide range of starting materials, including ketones, esters, hydrazones, and imines. Furthermore, the methods of the invention may be used in an asymmetric sense, i.e. to produce enantiomerically-enriched chiral α-aryl and α-vinyl products.

The invention belongs to the technical field of analysis and detection materials, and discloses an arylsalicylaldehyde-diphenyl-azine hydrazine compound as well as preparation and application. The compound has a structural general formula of formula (1) shown in the description, wherein Ar represents an aryl group or a derivative structure thereof, and substituent groups R1 to R10 are respectively selected from hydrogen, alkyl, alkoxy, aryl group and relative derivative structures thereof. The preparation method of the compound comprises the following steps: heating diphenyl hydrazine derivative and arylsalicylaldehyde to be 30 to 90 DEG C in a solvent for 6 to 12 hours' reaction, and separating and purifying reaction products, so as to obtain the arylsalicylaldehyde-diphenyl-azine hydrazine compound. The compound provided by the invention shows strong characters of a fluorescence probe, and also shows stronger selective recognition capability to substructures and metal ions in a cell, thereby achieving great high development value.

The invention relates to a Schiff base compound and a method for detecting an aniline compound thereof, belonging to the technical field of chemical sensor materials. The Schiff base compound is characterized by being prepared in such a way that an aromatic aldehyde compound with ortho-position hydroxyl reacts with monoamine or polyamine and has the structural formula shown as the figure, wherein n1 is an integer from 1 to 100, and n2 is an integer from 1 to 6; R is an aliphatic hydrocarbon substituted group, an aryl substituted group, heteroatom-substituted aliphatic alkyl or heteroatom-substituted aryl alkyl; and R1 and R2 are electron-withdrawing groups or electron-donating groups. The compound has stable solid fluorescence luminous performance, the fluorescence strength of the compound is changed by the aniline compound, the aniline compound can be detected according to the change of the fluorescence strength of the compound, and the compound is a novel fluorescence sensing material for detecting aniline.

On the basis of the current situation of self-repairing polyurethane materials, the invention provides an aromatic terminal hydroxyl chain extender containing an acylhydrazone bond, self-repairing polyurethane prepared by using the aromatic terminal hydroxyl chain extender and a preparation method of the self-repairing polyurethane. Compared with dihydric alcohol containing an acylhydrazone bond, the aromatic terminal hydroxyl chain extender containing the acylhydrazone bond has the advantages that the molecular structure of the aromatic terminal hydroxyl chain extender has the large pi bond of a hydrazide benzene ring and the pi-pi conjugative effect of the pi bond of carbon-oxygen double bonds, and accordingly the chain extender is stable in structure. The prepared self-repairing polyurethane has the advantages that the molecular chain of the polyurethane contains the reversible acylhydrazone bond, can achieve self-repairing under room temperature, and is high in repairing efficiency and good in mechanical performance. The preparation of the self-repairing polyurethane has the advantages that the method is simple, raw materials are products which are commercially produced, and the prepared polyurethane is high in performance controllability and promising in application prospect.

The invention discloses a STAT3 small-molecule inhibitor and its application, and the STAT3 inhibitor takes an N'-(1-(2,4 dihydroxy phenyl)ethylidene) benzoyl hydrazine derivative or its pharmacologically acceptable salt shown in a formula (1) or a formula (1a) as an effective component. In the formula, R1 and R2 on A ring can be hydroxyl, methoxy carboxyl and ester, and B can be an annular or a chain state. The STAT3 small-molecule inhibitor has selectivity and high activity, According to a three-grade structural design, biosynthesis and reconstructing optimization of STAT3, then a fluorescence polarization method and a CCK-8 method are employed for detecting activity and researching the mechanism on inhibition of tumor cells growth and promotion of differentiation apoptosis, so that effect of the STAT3 small-molecule inhibitor on prevention and control of tumor formation and tumor treatment can be described.

The invention discloses an aggregation-induced emission-based copper ion detection probe and a preparation method and application thereof. The structure of the fluorescent probe is as shown in a formula I, and the fluorescent probe is prepared through formylating hydroxytetrstyrene as a raw material and forming triphenylethylene-based salicylaldehyde azine together with hydrazine hydrate. The probe is stable in optical property, high in copper ion detection sensitivity and low in lower detection limit, the detection limit is 30.9nM and the response range is 0.5-7.5muM; the probe is good in selectivity and free of response to cations such as a silver ion, a barium ion, a calcium ion, a lithium ion, a magnesium ion, an ammonium ion, a nickel ion, a zinc ion, a mercury ion, a cobalt ion and a lead ion; and the probe is simple in synthesis, mild in condition and high in yield. The fluorescent molecular probe has practical application value in the field of copper ion detection in biochemistry and environmental chemistry.

The invention provides an anion receptor based on nitrophenylhydrazone and phenolic hydroxyl groups. The anion receptor is prepared by the following steps: 2, 6-diformyl-4-irgasan and paranitrophenylhydrazine are added into a reactor according to the quantity ratio of between 1 to 2 and 1 to 2.5, paratoluenesulfonic acid which accounts for 0.001 to 0.01 percent of the total mass of reactants is added as a catalyst, absolute ethyl alcohol which is 20 to 40 times of the total mass of the reactants is added as a solvent, and the reflux is performed for 3 to 6 hours at a temperature of between 70 and 100 DEG C to generate an orange precipitate; and the mixture is cooled to room temperature, and then the precipitate is filtered, is scrubbed by the absolute ethyl alcohol, and is recrystallized by DMSO to obtain the anion receptor. The anion receptor has the colorimetric identification ability to fluoride ions, acetates and dihydrogen phosphates in a DMSO solution, and has the selective colorimetric detection ability to acetate ions in DMSO / H2O solution. Anion detection test paper prepared by absorbing the anion receptor on the pretreated filter paper and drying the filter paper is used for colorimetric detection of the fluoride ions, the acetates and the dihydrogen phosphates, and has the characteristics of convenience for carrying, convenient use, high detection sensitivity and so on.

The invention relates to detection of a fluorescence method on metal ions, and particularly relates to a benzoyl hydrazine derivative P which identifies and detects two different metal ions Mg<2+> andAl<3+> separately in different pH conditions. The structural formula of the benzoyl hydrazine derivative P is as shown in a formula (1). The preparation method of the benzoyl hydrazine derivative P comprises the following steps: firstly, carrying out hydrazinolysis on ethyl salicylate; carrying out a reaction with o-hydroxy naphthaldehyde at a molar ratio of 1 to 1 for 4 hours at 80 DEG C in anhydrous ethanol; cooling the mixture and separating out a solid and carrying out suction filtration; washing the mixture with a lot of water and anhydrous ethanol successively; and drying the solid to obtain a light yellow solid pure product P. The benzoyl hydrazine derivative P can be used for detecting Mg<2+> and Al<3+> separately in different pH conditions as a fluorescent probe. The benzoyl hydrazine derivative P is obtained by means of an effective synthetic means and shows relatively good selectivity on the metal ions Mg<2+> and Al<3+> separately. On a basis of an optimized experimental condition, the metal ions Mg<2+> and Al<3+> can be detected separately. The formula is as show in the description.

The present invention relates to copper-catalyzed carbon-heteroatom and carbon-carbon bond-forming methods. In certain embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-nitrogen bond between the nitrogen atom of an amide or amine moiety and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. In additional embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-nitrogen bond between a nitrogen atom of an acyl hydrazine and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. In other embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-nitrogen bond between the nitrogen atom of a nitrogen-containing heteroaromatic, e.g., indole, pyrazole, and indazole, and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. In certain embodiments, the present invention relates to copper-catalyzed methods of forming a carbon-oxygen bond between the oxygen atom of an alcohol and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. The present invention also relates to copper-catalyzed methods of forming a carbon-carbon bond between a reactant comprising a nucleophilic carbon atom, e.g., an enolate or malonate anion, and the activated carbon of an aryl, heteroaryl, or vinyl halide or sulfonate. Importantly, all the methods of the present invention are relatively inexpensive to practice due to the low cost of the copper comprised by the catalysts.

The invention discloses a novel compound used as Cu<2+> colorimetric identification reagent, a preparation method and application of the compound. The novel compound is salicylidenehydrazine receptor obtained by condensing salicylaldehyde and hydrazine hydrate. The inventive compound with good metal ion identification ability can selectively identify Cu<2+>. Photochemical colorimetric probe prepared by the receptor can be widely applied to the technical field of heavy metal ion identification and detection.

The invention provides a long-chain p-nitrobenzoylhydrazone gelator. One side of the gelator is three long alkyl chains which have 16 C and are obtained through etherification, and the three long alkyl chains can form initial driving force for gelation through mutual action among carbon hydrogen; middle -NH obtained through a hydrazinolysis reaction can form stable gel with -CH and C=O adjacent to -NH through action of intermolecular hydrogen bonds and can also form corresponding binding sites with metal ions through coordination so as to further form the organic metal gel; the formed organic metal gel can realize rapid highly-selective fluorescent recognition of I<-> in water and is obvious in color changes, which enables detection with the naked eyes to be conveniently and rapidly realized; and the formed organic metal gel has good stability, is easy to store and carry and convenient to use and can be used for writing and storage of confidential materials.

The invention discloses a fat soluble dual-core cobalt (III) anti-tumor coordination compound and a preparation method thereof. The fat soluble dual-core cobalt (III) anti-tumor coordination compound belongs to lipophilic cobalt anti-tumor coordination compounds. The coordination compound of the invention has a chemical name of N,N'-bis(salicylidene)diamine cobalt (III) ([Co2(C14H12N2O2)3] for short), a molecular formula of C42H33Co2N6O6 and a molecular weight FW of 834.63, and is prepared by using CoAc2.4H2O as a raw material and by the steps of performing a quantitative reaction of the CoAc2.4H2O and ligand N,N'-bis(salicylidene)diamine in a solvent of dimethyl formamide and separating out products. The anti-tumor activity of the coordination compound is 1.6 times that of cis-platinum and 5 times that of carboplatin; an anti-tumor G150 value is 0.35mu g / mL; the activity is higher than those of the cis-platinum and carboplatin; and the coordination compound is low in toxicity and high in fat solubility and is used for clinical tumor treatment.

The invention belongs to the technical field of medicinal chemistry, and in particular relates to acylhydrazone compounds with anti-tumor activity as well as a preparation method and application of the acylhydrazone compounds. The structures of the acylhydrazone compounds are as shown in a general formula (I) shown in the description, wherein R and R' are independently selected from any one or more of halogen, amino, cyano, alkoxy, 3,4-methylenedioxy, nitro, phenyl or substituted phenyl, and R and R' substituents are mono-substituted, disubstituted or tri-substituted. The preparation method issimple; biological activity test results of the compounds show that the compounds have a very good inhibitory effect on histone methyltransferase SET7, and have good application prospect in the development of anti-tumor aspects.

The invention discloses an organic bi-metal gel capable of recognizing cyanic group ions through a fluorescent colorimetric method. The gel is prepared by dissolving a gelator, namely 1-naphthyl-3,4,5-tri(hexadecyloxyl) benzoyl hydrazone, Ca<2+>, and Cu<2+> into an organic solvent, and cooling to the room temperature so as to form the organic bi-metal gel. When negative ions are added into the organic bi-metal gel, only CN<-> can convert the color of the organic bi-metal gel from dark green to tawny, and very strong fluorescence is generated at the same time; other negative ion aqueous solution do not change the color of the organic bi-metal gel, and no fluorescence is generated; so the organic bi-metal gel can recognize the CN<-> in water liquid through a fluorescent colorimetric method in a mono-selectivity way, so that a person can quickly and conveniently detect CN<-> in water through his naked eyes.

The invention belongs to the technical field of organic synthesis and discloses a trifluoroacetyl substituted hydrazone derivative and a synthesis method thereof. The trifluoroacetyl substituted hydrazone derivative has a structural formula shown as a formula (I); the synthesis method of the trifluoroacetyl substituted hydrazone derivative comprises the following steps: adding diazotate, trifluoromethyl ketone, alkali and a solvent into a reactor; stirring and reacting at 0 to 70 DEG C for 0.05 to 24h; after reaction is finished, cooling to room temperature; adding water and an organic solventand extracting a reaction solution; evaporating to remove the solvent, so as to obtain a crude product; and carrying out column chromatography purification to obtain the trifluoroacetyl substituted hydrazone derivative. The synthesis method provided by the invention does not utilizes a catalyst and does not need a ligand, and all raw materials have no toxicity and are cheap and easy to obtain; the reaction has good adaptability on functional groups, wide substrate adaptability and high product yield; and the synthesis method is simple and safe to operate and has moderate reaction conditions and a good industrial application prospect. The formula (I) is shown in the description.

The invention provides a dihydroxybenzoylhydrazone neuraminidase inhibitor and preparation and application thereof. The neuraminidase inhibitor is characterized by adopting a structural formula as shown in the description. The neuraminidase inhibitor has excellent anti-H1N1 influenza virus activity, adopts a structure completely different from that of previous neuraminidase, has a good effect of inhibiting A / WSN / 33H1N1 virus strain, is less in toxicity and has high druggability.

The invention discloses an o-nitrophenyl azo salicylaldehyde phenoxy acetyl hydrazone compound. According to the o-nitrophenyl azo salicylaldehyde phenoxy acetyl hydrazone compound, the compound is prepared through taking anhydrous ethanol as a solvent, glacial acetic acid as a catalyst and o-nitrophenyl azo salicylaldehyde and phenoxy acethydrazide as reaction substrates, carrying out reflux reaction until precipitates are produced, standing, and carrying out suction filtration and recrystallization; the role of the compound in recognition on negative ions, such as F<->, Cl<->, Br<->, I<->, CH3COO<->, H2PO4<->, HSO4<->, ClO4<-> and CN<->, is inspected through ultraviolet-visible absorption spectrum, colorimetric recognition and <1>HNMR titration; and shown by results, the compound can carry out high-selectivity colorimetric recognition on CN<-> in a DMSO (Dimethyl Sulfoxide) water-bearing system. CN<-> detection test paper manufactured based on a receptor, namely the compound, can be used for detecting cyanogens ions conveniently and fast. Thus, receptors of the type have a certain potential application value in the colorimetric detection on CN<-> in water-bearing systems.

The invention designs and synthesizes an acceptor 1-(3,4-bis(hexadecyloxy)benzylidene)2-(-4-nitrophenyl) hydrazon capable of colorimetrically identifying fluorine ions with high selectivity. The acceptor has a single-selectivity colorimetric identifying capacity to the fluorine ions in DMSO (dimethylsulfoxide) solution. The acceptor is heated and dissolved in DMSO or DMF (Dimethyl Formamide) to prepare solution with the mass concentration of 0.6-2.0%, and the solution is cooled to the room temperature to form the stable organogel, wherein the color of the organogel is changed from saffron to reddish brown when the organogel comes into contact with fluorine ion solution and is not changed when comes into contact with other ion solutions. Therefore, being an intelligent supermolecule gel material for identifying the fluorine ions with single selectivity, the acceptor can be used for colorimetrically identifying the fluorine ions with high selectivity conveniently and quickly at low cost.

The invention provides a benzoyl hydrazone neuraminidase inhibitor. The inhibitor is characterized in that the structure of the inhibitor is shown in the formula I. The inhibitor has the advantage that according to the structural formula, the synthesized compound has good neuraminidase inhibiting activity.

A provided synthetic method for an intermediate of benserazide hydrochloride comprises the following steps: step (a), taking DL-serine and thionyl chloride as initial raw materials, reacting to generate methyl-DL-serine hydrochloride, concentrating the reaction solution to dry, so as to obtain serine methyl ester, dissolving with methanol for usage in the reaction of step (b); step (b), adding serine methyl ester obtained in the step (a) into hydrazine hydrate, after reaction is finished, adding an alcohol, and adjusting ph to crystallize and further to obtain serine hydrazide; and step (c), reacting serine hydrazide obtained in the step (b) with 2,3,4-trihydroxybenzaldehyde in a methanol system, so as to obtain N-(DL-seryl)-2,3,4-trihydroxybenzaldehyde hydrazone. The preparation method disclosed by the invention is high in yield, low in cost, short in reaction period, environment-friendly and suitable for industrialized production.

The invention discloses a method for synthesizing prothioconazole and an optical active body thereof and an intermediate. According to the method, a hydrazine compound and glyoxylic acid react to obtain a hydrazono acetic acid intermediate, and then the hydrazono acetic acid intermediate reacts with thiocyanate to obtain a prothioconazole target product. The reaction regioselectivity is good, few side products are generated, and the yield is high. The requirement for equipment is not high, and anhydrous and anaerobic operation is not needed. The process is simple, few three wastes are generated, and the method is suitable for industrial production.

The invention discloses a formula and a production process for preparing methyl ethyl ketazine by utilizing a hydrogen peroxide method, which carries out an in-depth study on the hydrogen peroxide method, thereby improving the hydrogen peroxide method to form a ketazine production method suitable for the situations in China. In the method, hydrogen peroxide is used as an oxidant, ammonia and butanone (methyl ethyl ketone) are used as raw materials and formamide and an inorganic oxide are used as a catalyst and a cocatalyst respectively to interact with each other so as to prepare the ketazine, wherein the hydrogen peroxide belongs to an industrial product and has the concentration of 25% to 30%; ammonia is added in a form of ammonia water with the concentration of 20% to 25%; and the butanone, the formamide and the inorganic oxide are all in the industrial product level. The method disclosed by the invention can be used for solving the problems that the existing initial coarse products for producing hydrazine hydrate are low in concentration, high in energy consumption, low in efficiency and high in cost and the by-products are difficult to treat, thereby being suitable for the situations in China.

The invention discloses an organic gel material and a preparation method thereof and belongs to the technical field of supramolecular self-assembly. Organic gel is obtained by dissolving a small-molecular compound 4-(3,4-(octaneoxy)phenyl)-pyrene carbonylhydrazone in a dimethyl sulfoxide solvent under the heating condition and then performing cooling to reach room temperature. The prepared organic gel has gathered and induced fluorescence enhancement properties and visible-light response. In addition, xerogel prepared based on the organic gel has a force-sensitive fluorescence phenomenon. The organic gel has the gathered and induced fluorescence enhancement properties and visible light and external force response and has the potential application prospect on the aspects of fluorescence switches, external force detection, sensors and the like.

The invention discloses a method for synthesizing ketazine by a hydrogen peroxide oxidation method. The ketazine is synthesized by using ketone and ammonia as raw materials, hydrogen peroxide as an oxidant and acetamide-ammonium acetate-Na2HPO4 as a catalyst. The method is characterized in that: an extracting agent is added into a reaction system, wherein the extracting agent is an organic solvent which is soluble in the ketazine and insoluble in water, such as alkane of cyclohexane, n-hexane, n-heptane and the like, and halogenated hydrocarbon of chloroform, 1,2-dichloroethane, 1,1,1-trichloro ethane, carbone tetrachloride and the like; and one or more of the alkane and the halogenated hydrocarbon can be added. The method has high yield of products and the extracting agent can be recycled.