88results about "Hydrazone preparation" patented technology

The invention provides a preparation method of apixaban, and belongs to the technical field of raw material medicine synthesis. The intermediate product 5 is prepared by adopting continuous flow equipment, so that the defect of low heat and mass transfer efficiency of an intermittent reaction kettle is overcome, the reaction danger coefficient is reduced, the reaction time is shortened, the product quality is improved, and the product yield is increased; a ferric trichloride / activated carbon-hydrazine hydrate system is adopted for nitro reduction, so that the selectivity is good, and the product purity and yield are improved; the ethanol solution of ammonia is adopted to replace ammonia water, CH3ONa / HCOONH2, mixed anhydride-ammonia water and the like in the prior art, the defects that in the prior art, the content of acid impurities is high, and the amount of post-treated ammonia-containing wastewater is large are overcome, and the environmental protection pressure is reduced while the product quality is improved.

The invention discloses an antibacterial bioactive glass composite material for skull defect repair and a preparation method thereof, and relates to the technical field of bioactive glass materials. The antibacterial bioactive glass composite material for skull defect repair is prepared from the following raw materials in parts by weight: 8 to 15 parts of collagen, 45 to 55 parts of bioactive glass, 20 to 30 parts of hydroxyapatite, 5 to 8 parts of a toughening agent, 1 to 2 parts of an antibacterial agent and 150 to 250 parts of deionized water. The antibacterial bioactive glass composite material for skull defect repair prepared by the invention has excellent bending strength and antibacterial property.

The invention discloses a synthetic method of methyl ethyl ketazine, which comprises the following steps: taking a cyano covalent organic framework material as a solid catalyst, taking butanone and ammonia water as raw materials, taking a hydrogen peroxide solution as an oxidizing agent, adding a certain amount of dimethyl sulfoxide (DMSO) and inorganic base, and reacting at a certain temperature to synthesize the methyl ethyl ketazine. According to the method, the catalyst is easy to separate, recover and recycle, and the yield of methyl ethyl ketazine is high.

The present invention proposes a method and use for stabilizing a simple agglomerate for pH and salt and with adjustable size. In phosphoric acid buffer solutions with different salt concentrations and pH values, the polyacrylic acid hydroxypropyl group condensation body has specific stability; hydrophobic thermal response blocks are introduced into a hydroxypropyl acrylate monomer through reversible addition-fragmentation chain transfer polymerization to regulate and control the size of a condensation body, and a phase separation behavior is shown at different temperatures; a hydrophobic block without thermal response is introduced to regulate and control the size of the aggregate, and no thermal response behavior is shown. Continuous regulation and control of the size of the aggregate from the micron level to the nano level are achieved, and the requirements of different application scenes are met. The hydroxypropyl polyacrylate condensation body can be used for packaging various dyes and drugs; high-efficiency enzyme protection is achieved, formed aggregates can protect glucose oxidase, and the retention rate of enzyme activity reaches 85% or above after treatment is conducted for 3 hours at 60 DEG C; as a micro-reactor for the reaction of generating p-nitrobenzaldehyde phenylhydrazone from p-nitrobenzaldehyde and phenylhydrazine, the reaction rate is greatly improved.

Provided is a polymerizable liquid crystal compound represented by general formula (I). [In general formula (I), J1 represents a monovalent group represented by general formula (J-1), and the symbols in general formula (I) and general formula (J-1) are as defined in the description.]

The invention belongs to the field of chemical medicine synthesis, and particularly relates to an acylhydrazone compound, a preparation method thereof and application of the acylhydrazone compound in camellia oleifera anthracnose and soft rot. The structure of the acylhydrazone compound is shown as a formula I, and the acylhydrazone compound is directly prepared from citronellal and formylhydrazine through a one-step reaction. The invention provides the acylhydrazone compound, the IC50 of the acylhydrazone compound on liver cancer can reach 7.0 mu M, and a new solution is provided for research and development of drugs for treating liver cancer. The EC50 (mg / L) of the strain can reach 1.65 when the strain is used in an oil-tea camellia anthracnose strain inhibition experiment, the EC50 (mg / L) of the strain can reach 1.38 when the strain is used in an oil-tea camellia soft rot strain inhibition experiment, and a new solution is provided for controlling oil-tea camellia anthracnose and soft rot. Meanwhile, the invention provides a synthesis method of citronellal and formylhydrazine through one-step reaction, and the synthesis method has the advantages of high yield, high raw material conversion rate, high selectivity and the like. And the formula I of the # imgabs0 # is shown in the specification.

The invention provides an aldehyde insect pheromone derivative, which takes a compound containing at least one primary amine group as a carrier, and aldehyde insect pheromone forms an imine derivative with the compound through chemical reaction. The invention also provides a preparation method, application and a release method of the aldehyde insect pheromone derivative. According to the aldehyde insect pheromone derivative provided by the invention, aldehyde insect pheromones are treated in a chemical reaction manner, the stability of the aldehyde insect pheromones can be remarkably improved, slow release and controlled release of the pheromones can also be realized, the carrier material is wide in source, more in selectivity, convenient and economical, and in addition, the aldehyde insect pheromone derivative has good application prospects. The aldehyde insect pheromone derivative provided by the invention can also realize combined fixation and release of various pheromones, so that trapping, prevention and control of various insects can be realized.

The invention relates to the field of biomedicine, and discloses a preparation method and application of an I-type composite photosensitizer with hydrogen sulfide detection performance. According to the invention, TPA-CHO and MN are adopted as monomers, a Schiff base reaction is adopted to synthesize a triphenylamine derivative TPAB with an A-pi-D-pi-A conjugated structure, Cu < 2 + > is further introduced into TPAB molecules, and a stable metal complex composite photosensitizer is formed through a coordinate bond. The functional composite photosensitizer TPAB-Cu < 2 + > has the characteristic of mainly generating I-type ROS and has efficient photodynamic bactericidal activity in an anoxic drug-resistant bacterium infection environment, and in addition, the functional molecule can be applied to drug-resistant bacterium infection microenvironment hydrogen sulfide level detection so as to realize early warning of drug-resistant bacterium infection and real-time detection of a treatment process; the technical problems that in an existing photodynamic therapy, the oxygen dependence of a photosensitizer is high, and the response sensitivity and specificity of a drug-resistant bacterium infection microenvironment are insufficient are solved.

The invention discloses a continuous flow synthesis method of diacetone hydrazone. The method comprises the following steps: S1, acetone and hydrazine hydrate are respectively pumped into a microchannel reactor for a mixed reaction, and the first retention time is 5.6-8.5 s; s2, the mixed liquid flowing out of the micro-channel reactor in the step S1 flows into a tubular reactor connected with the micro-channel reactor in series for continuous reaction, and the second retention time is 200-300 s; and S3, collecting the mixed liquid flowing out of the tubular reactor in the step S2. According to the invention, the micro-channel reactor and the tubular reactor which are sequentially connected in series are adopted for reaction, so that the defects of low efficiency, low purity of the obtained product, safety problem and the like in the traditional batch method are overcome, and the continuous flow synthesis method which is efficient, safe, rapid, economical and easy for large-scale production of diacetone hydrazone is provided.

This application relates to the biomedical field and discloses a method for preparing a type I composite photosensitizer with both hydrogen sulfide detection capabilities and its uses. The invention synthesizes a triphenylamine derivative TPAB with an A-π-D-π-A conjugated structure using TPA-CHO and MN as monomers via a Schiff base reaction, and further incorporates Cu... 2+ By introducing TPAB molecules, a stable metal complex photosensitizer is formed through coordination bonds. This application presents the functional composite photosensitizer TPAB-Cu. 2+ Characterized primarily by the generation of type I ROS, it exhibits highly efficient photodynamic bactericidal activity in hypoxic environments infected with drug-resistant bacteria. Furthermore, this functional molecule can be used to detect hydrogen sulfide levels in the microenvironment of drug-resistant bacterial infections, enabling early warning and real-time monitoring of the treatment process. This solves the technical problems of strong oxygen dependence of photosensitizers and insufficient sensitivity and specificity in response to the microenvironment of drug-resistant bacterial infections in existing photodynamic therapies.

A method for preparing the insecticide N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is disclosed. A method for preparing the intermediate N-(1-methylcyclopropyl)-2-(3-pyridinyl)-2H-indazole 4-carboxamide is also disclosed.

The utility model relates to the technical field of benzophenone hydrazone production, and discloses a proportioning device for producing benzophenone hydrazone, which comprises a barrel body, a control panel is arranged on the front side of the barrel body, a heat conducting plate is fixedly connected in the barrel body, the lower part of the heat conducting plate is fixedly connected with a motor, and the lower part of the heat conducting plate is fixedly connected with the motor. The output end of the motor is fixedly connected with a stirring assembly, the right side of the barrel body is fixedly connected with a supporting plate, the upper portion of the supporting plate is fixedly connected with an air extracting pump, the input end of the air extracting pump is fixedly connected with an air extracting pipe, the output end of the air extracting pump is fixedly connected with an air conveying pipe, and the left end of the air conveying pipe is fixedly connected with a heater. According to the reaction kettle, the raw materials in the barrel body are mixed, the reaction temperature can be controlled, the reaction is promoted, the reaction uniformity is ensured, the raw materials such as benzophenone and hydroxylamine are accurately added into the reaction kettle, and the accurate matching is ensured.

The invention discloses a method for synthesizing dihydrocapsaicin, and the method comprises the following steps: synthesizing a first intermediate 1-isobutylcyclohexene, a second intermediate 8-methyl-6-oxonanoic acid, a third intermediate 8-methylnonanoic acid and a target product dihydrocapsaicin. The method uses cyclohexanone, isobutylmagnesium bromide and vanillin ammonium hydrochloride as raw materials, and obtains the product dihydrocapsaicin by stepwise reaction. Each reaction step adopts a conventional chemical reaction, and the reaction conditions are mild. The feasibility of the synthesis process is high, the safety and environmental protection are strong, and the product has a high yield and good purity, and is suitable for industrial production.

The invention relates to the technical field of biurea preparation, in particular to a system and a method for continuously preparing biurea. According to the method, acetone, liquid ammonia, chlorine and urea are used as raw materials, a continuous flow reactor with a micro-channel reactor and a tubular reactor is used, biurea is generated by adopting an acetone azine process route, and the byproduct acetone and ammonia are directly recycled after being condensed and absorbed, so that the consumption cost of the raw materials is greatly reduced, the resource utilization rate is increased, and the method has outstanding economic benefits. According to the method, the high-risk ketazine synthesis reaction is limited in a channel with extremely small liquid holdup to be safely carried out at low temperature, the explosion risk caused by accumulation of nitrogen-containing intermediates is greatly reduced, inorganic acid and alkali metal salt are not introduced into the whole process, the process is green and environment-friendly, high-salinity wastewater is completely eradicated from the reaction principle, the most important pollution source is eliminated from the source, and the production cost is reduced. And the environmental protection advantage is extremely remarkable, and the most severe environmental protection difficulty of the traditional process is solved. And the process is green, environment-friendly, low in energy consumption and suitable for large-scale and automatic production.

The utility model discloses equipment for continuously preparing ketazine, which relates to the technical field of azodiisobutyronitrile production and comprises a hydrazine hydrate feeding jacketed pipe, an acetone feeding jacketed pipe, a sectional tubular reactor and a ketazine storage tank, the hydrazine hydrate feeding jacketed pipe and the acetone feeding jacketed pipe are both communicated with a material inlet of the sectional type tubular reactor, a material outlet of the sectional type tubular reactor is communicated with a feeding port of the ketazine storage tank, and the ketazine storage tank comprises a jacket cooling system. Compared with the traditional kettle type reaction method, the reaction time is shortened to 1-1.5 hours, the equipment structure is simple, the utilization efficiency of unit volume is greatly improved, the volume of the reactor is reduced, the safety level is essentially improved, the reaction proportion is more accurate, and the conversion rate is improved by 0.8%-1.5% compared with the traditional method.

The application belongs to the technical field of organic synthesis, and particularly relates to a method for efficiently and greenly preparing allyl ketoxime in one step. The preparation method specifically comprises the following steps: cross-coupling reaction of enol, hydrazine and aldehyde under the action of a palladium catalyst to obtain an allyl ketoxime compound. The reaction raw materials used in the application are cheap and easy to obtain. The allyl ketoxime compound can be efficiently and greenly prepared in one step through the coupling reaction, the synthesis process is simple, and the synthesis cost is greatly reduced. The reaction condition is mild, the yield is high, the substrate applicability range is wide, the reaction conversion efficiency is high, the gram-scale experiment can be realized, and industrialization is easy to realize.

The application discloses a kind of photo-curing mussel biomimetic acylhydrazone and its preparation method and application, the structural formula of the photo-curing mussel biomimetic acylhydrazone is as shown in formula (I).The photo-curing mussel biomimetic acylhydrazone of the application has catechol structure and carbon-carbon double bond, raw material is low in price, synthesis process does not need to modify catechol structure, preparation method is simple, can reduce the synthesis difficulty and production cost of mussel biomimetic material.The mussel biomimetic photo-curing adhesive composition prepared by using photo-curing mussel biomimetic acylhydrazone as raw material has good adhesive property, and can improve the problem of insufficient adhesion and failure of photo-curing adhesive, and prevent falling.

The invention relates to acylhydrazone molecules capable of activating solid-state fluorescence or photochromism and preparation and application thereof, in the molecular structure, by changing a substituent R on a-N (R)-group on one side of benzoyl hydrazine, the conformation and accumulation mode of the molecules can be adjusted, so that selective activation of the fluorescence or photochromism property of the acylhydrazone molecules in a solid state is realized. When the substituent R is-H, the molecular conformation is planar, and the intermolecular accumulation is tight. In a solid state, the compound shows an excitation wavelength dependent fluorescence property, and when the wavelength of excitation light is changed, the fluorescence color is switched between blue and green. When the substituent R is-CH3, due to the steric effect of-CH3, the molecular conformation is distorted, and the accumulation among molecules becomes more loose. When ultraviolet light and visible light are alternately used for irradiation in a short time, the color of the powder can be rapidly switched between white and orange. The method provided by the invention is not influenced by R'on a benzene ring, and shows good universality.

Processes for preparing (((3aR,6aS)-5-(4,6-dimethylpyrimidin-2-yl)hexahydropyrrolo[3,4-c]pyrrol-2(1H)-yl)(2-fluoro-6-(2H-1,2,3-triazol-2-yl)phenyl)methanoneare described, which are useful for commercial manufacturing. Said compound is an orexin receptor modulator and may be useful in pharmaceutical compositions and methods for the treatment of diseased states, disorders, and conditions mediated by orexin activity, such as insomnia and depression.

The invention relates to a synthesis method of a benzoyl hydrazone derivative and an antitumor activity research of the benzoyl hydrazone derivative. A series of benzoyl hydrazone derivatives are synthesized by modifying benzamide and hydrazone. The synthesis method is simple, convenient and efficient, and has better selectivity and yield. In-vitro cell experiments show that the synthesized derivatives have remarkable anti-tumor activity, and especially in the aspect of inhibiting the growth of U87 (human brain astroblastoma cells), SGC-7901 (human gastric cancer cells) and HepG2 (human liver cancer cells), part of the derivatives show a low nanomole-level IC50 value. Researches show that the benzoyl hydrazone derivatives may play an anti-tumor role by inhibiting tumor cell proliferation, inducing apoptosis and other mechanisms, and have the potential to become novel anti-tumor drugs. The synthesis method of the compound, the antitumor activity and the mechanism research of the compound provide effective thinking and basis for developing new antitumor drugs, and the compound has a wide application prospect.

The invention provides a preparation method of hydrazine hydrate, which comprises the following steps: in the presence of a catalyst and under reaction conditions, introducing methyl ethyl ketazine and water into a reaction section of a composite rectifying tower for contact reaction, and then continuously producing a hydrazine hydrate solution from a tower kettle. The preparation method of hydrazine hydrate provided by the invention can catalytically hydrolyze methyl ethyl ketazine under low-temperature and low-pressure reaction conditions, and meanwhile, the concentration and yield of hydrazine hydrate are improved.

The invention discloses a fully continuous flow chemical synthesis method of an apixaban intermediate (Z)-2-chloro [(4-methoxyphenyl) hydrazono] ethyl acetate. The fully continuous flow chemical synthesis method comprises the following steps: introducing a sodium nitrite solution, a solution of a compound as shown in a formula (I) and acid into a dynamic tubular reactor, and carrying out diazotization reaction under the condition that the temperature is not higher than 0 DEG C; and introducing a sodium acetate solution and an ethyl 2-chloroacetoacetate solution into the microchannel reactor, mixing with the diazotization reaction solution, carrying out a Jappp-Klingemann reaction at-5-2 DEG C, and concentrating to obtain the apixaban intermediate compound shown in the formula (II). The invention provides a full-continuous flow chemical synthesis method of an apixaban intermediate (Z)-2-chloro [(4-methoxyphenyl) hydrazono] ethyl acetate. The target product can be efficiently prepared in dozens of seconds in a high-purity and high-yield manner.

The invention belongs to the technical field of biological medicine, and particularly relates to a Schiff base vanillin acetylcholin esterase inhibitor and a preparation method and application thereof, the Schiff base vanillin acetylcholin esterase inhibitor has a structure shown as a formula (I): # imgabs0 #, in the formula (I), R1 is phenyl connected with a substituent group, and R2 is a group containing carbonyl, sulfuryl or heterocyclic ring. Compared with the prior art, the invention provides the acetylcholin esterase inhibitor with a novel structure, and experiments show that the acetylcholin esterase inhibitor has good acetylcholin esterase inhibition activity and can be used for preparing medicines for inhibiting the acetylcholin esterase activity.

The invention relates to the technical field of chemical synthesis, in particular to a recovery method and application of a methyl ethyl ketazine working solution, the methyl ethyl ketazine working solution comprises an amide catalyst, an acid ammonium catalyst and water, and the recovery method of the methyl ethyl ketazine working solution comprises two steps: S1, concentration of a methyl ethyl ketazine synthesis reaction solution; s2, the methyl ethyl ketazine working solution is recycled, the target product methyl ethyl ketazine and the recycled methyl ethyl ketazine reaction solution are finally obtained, the tubular reactor is utilized in the methyl ethyl ketazine working solution recycling process, rapid and efficient recycling of the methyl ethyl ketazine working solution is achieved, and compared with an existing methyl ethyl ketazine working solution recycling mode, the reaction efficiency is remarkably improved, and the production cost is reduced. The treatment time is greatly shortened, the method is easier to realize industrial amplification and production, and an innovative and practical technical scheme is provided for efficient synthesis of methyl ethyl ketazine and recovery of the catalyst.

The present invention relates to an improved synthetic process for the preparation of (2H-1, 2, 3-triazol-2-yl) phenyl compounds as orexin receptor modulators. The present invention describes a process for the preparation of (((3aR, 6aS)-5-(4, 6-dimethylpyrimidin-2-yl) hexahydropyrrolo [3, 4-c] pyrrol-2 (1H)-yl) (2-fluoro-6-(2H-1, 2, 3-triazol-2-yl) phenyl) ketone # imgabs0 #, which can be used in commercial manufacturing. The compounds are orexin receptor modulators and are useful in pharmaceutical compositions and methods for treating disease states, disorders, and conditions mediated by orexin activity, such as insomnia and depression.

This application provides a positive electrode additive and its preparation method, a positive electrode sheet, a secondary battery, and a battery pack, wherein the positive electrode additive includes a fluorohydrazone compound represented by Formula I or Formula II. In Formula I, R1, R2, and R3 are each independently selected from -H or -F, and R1, R2, and R3 are not simultaneously -H; R4 is selected from substituted or unsubstituted alkyl, halogen, or nitro groups. In Formula II, R5, R6, and R7 are each independently selected from -H or -F, and R5, R6, and R7 are not simultaneously -H; R8 is selected from substituted or unsubstituted alkyl, halogen, or nitro groups.

The application provides an EGFR / HER2 inhibitor based on a hydrazone structure, a preparation method and application thereof, and belongs to the field of medicines; specifically provides a hydrazone derivative, which has a chemical structural formula as shown in formula A, wherein R is a methyl group or a hydrogen group, and X is halogen, a hydroxyl group or a methoxyl group; and a preparation method of the hydrazone derivative is provided; the hydrazone derivative provided by the application has an antitumor effect as an EGFR and / or HER2 inhibitor, and can be used for preparing an antitumor drug. Formula A

The invention discloses a preparation method of amide COF and application of the amide COF in methyl ethyl ketazine synthesis. The preparation method of the amide COF comprises the following steps: mixing a cyano COF material with H2O2, inorganic alkali, dimethyl sulfoxide (DMSO) and methanol, carrying out a reaction under a stirring condition, carrying out centrifugal separation on a reaction product, washing a precipitate with ultrapure water, and carrying out vacuum drying to obtain the amide COF material. The synthesized amide COF material has high catalytic activity and good selectivity in the synthesis of methyl ethyl ketazine, is easy to separate and can be recycled.

The present invention discloses a supramolecular sensor based on pentafluorophenyl functionalized tetrapod azine, which is obtained by using pentafluorobenzaldehyde and 4,4'-biphenyl diphenol tetrahydrazine derivative as reaction substrates. In DMSO solution, the sensor TF5 can undergo supramolecular interaction with perfluorooctanoic acid and fluorescence enhancement occurs at the same time, so it can be used for fluorescence recognition of perfluorooctanoic acid, with a minimum detection limit of 9.27×10 ‑6 M, the sensor TF5 has important application value in the field of detecting perfluorooctanoic acid.

The present invention addresses the problem of providing a novel crystal. A crystal of 3-hydroxy-N'-(1, 3-dimethylbutylidene)-2-naphthoic acid hydrazide which has a peak with the maximum intensity at a diffraction angle (2θ) of 6.1 ± 0.2° in the powder X-ray diffraction pattern.