198 results about "Succinchlorimide" patented technology

The invention discloses a preparation method of a cell inflammatory factor adsorbent, which comprises the following steps: mixing styrene, divinyl benzene and hydroxyethyl acrylate, and adding a pore-foaming agent and mesoporous SiO2 nano powder to prepare a porous microsphere carrier; the preparation method comprises the following steps: mixing chitosan and poly (N-isopropylacrylamide) in an acetic acid solution to obtain a temperature-sensitive chitosan hydrogel precursor solution; the preparation method comprises the following steps: activating the surface of a porous microsphere carrier by using 1-ethyl-(3-dimethylaminopropyl) carbodiimide and N-hydroxysuccinimide, mixing the activated porous microsphere carrier and a temperature-sensitive chitosan hydrogel precursor solution to obtain a water phase, and assembling, washing and drying in an oil phase to obtain the cell inflammatory factor adsorbent. Through the design of the core-shell structure and the addition of the mesoporous SiO2 nano powder, the temperature response characteristic and the recyclable characteristic are given to the cell inflammatory factor adsorbent, the adsorption capacity of cell factors is also improved, and a new solution is provided for physical adsorption of the cell inflammatory factors.

The invention relates to the technical field of protective films, in particular to a high-light-transmittance label protective film and a preparation method thereof.A multi-layer protective film formed by compounding a release film layer, an adhesive layer, a PET film and a protective layer is constructed; composite vinyl ester resin constructed by taking epoxy resin and acrylic acid as raw materials is subjected to toughening modification, and then a linear reactive diluent is compounded to construct a high-toughness protective layer which is resistant to high temperature and aging and can be photo-cured; long-chain alkane modified nano silicon dioxide is introduced into the protective coating, nano silicon dioxide is aminated by 3-aminopropyltriethoxysilane, and then 17-carbon monoisocyanate prepared by taking acetone, stearic acid, triphenylphosphine, sodium azide and N-chlorosuccinimide as raw materials is grafted to form the long-chain alkane modified nano silicon dioxide. Vinyl butadiene styrene rubber, composite vinyl ester resin, tackifying resin, a softening agent and a photoinitiator are mixed to prepare the adhesive layer.

The invention discloses a C60-BODIPY triplet photosensitizer as well as a preparation method and photodynamic antibacterial application thereof. In the preparation process, a fullerene pyrrole ring compound and a BODIPY molecule are connected together through a benzene bridge group, and two ends of a bridge bond are respectively connected to a C atom on a fullerene pyrrole ring and a 6th site of the BODIPY molecule; a BODIPY-C60 binary molecule is formed; the preparation method comprises the following steps: reacting 9-anthracene formaldehyde with 2, 4-dimethyl pyrrole to generate a boron-dipyrromethene molecule of which the meso position is substituted by 9-anthryl, brominating the boron-dipyrromethene molecule at the 6 position by N-bromosuccinimide, coupling the boron-dipyrromethene molecule with p-formylphenylboronic acid, and carrying out Prato reaction on the coupled boron-dipyrromethene molecule with C60 and N-methylglycine to prepare the BODIPY-C60 binary triplet photosensitizer. The triplet photosensitizer has excellent photodynamic activity and relatively high reactive oxygen quantum yield, and can effectively kill bacteria.

The invention relates to the field of coatings, and discloses a self-cleaning nano-coating glass plate and a preparation method and application thereof.The nano-coating is prepared from organic silicon resin, epoxy resin, modified nano titanium dioxide, long-chain alkyl methyl silicone oil, a curing agent and a diluent; the modified nano titanium dioxide is prepared by grafting a modified silane coupling agent and nano titanium dioxide, wherein the modified silane coupling agent is prepared by reacting a modified phosphorus-containing antibacterial monomer with vinyltriethoxysilane; the modified phosphorus-containing antibacterial monomer is prepared by reacting eugenol with N-bromosuccinimide, then reacting with 2-amino-4-methylthiazole, further reacting with diphenyl phosphinyl chloride, and reacting the obtained phosphorus-containing antibacterial monomer with 1, 1, 3, 3-tetramethyldisiloxane; the long-chain alkyl methyl silicone oil is prepared by using octamethylcyclotetrasiloxane, dodecyl methyl dimethoxy silane and hexamethyldisiloxane as raw materials, and the prepared nano coating has a super-hydrophobic surface and also has excellent antibacterial activity, wear resistance and flame retardance.

The present invention relates to a method for preparing a sulfonepyraclostrobin intermediate, comprising the following steps: S1, in a solvent, acetic acid oxime and N-chlorosuccinimide react to obtain a reaction solution containing dichloroformaldehyde oxime; S2, in water, under the action of a catalyst and a base, dichloroformaldehyde oxime and isobutylene in the reaction solution obtained by S1 react, and after the reaction is completed, 3-chloro-5,5-dimethyl-4,5-dihydroisoxazole is obtained by post-treatment. The present invention produces 3-chloro-5,5-dimethyl-4,5-dihydroisoxazole at a higher yield on the basis of using acetic acid oxime, with the advantages of reducing reaction temperature, improving reaction yield, effectively controlling side reactions, and realizing greater economic benefits.

The invention discloses a high-performance clean type anti-wear hydraulic oil complexing agent which is prepared from the following substances in parts by mass: 30 to 60 parts of an antioxidant, 20 to 40 parts of an anti-wear agent, 2 to 5 parts of boronized polyisobutylene bis-succinimide, 2 to 7 parts of thiocarbamate, 4 to 10 parts of dodecenylsuccinic acid and 0.2 to 2 parts of graphene nanosheets. The lubricating oil is prepared from the following components in parts by weight: 0.5-1.5 parts of a metal deactivator, 0-2 parts of DISUPER S24 and 30-50 parts of base oil. The preparation method comprises the following steps: S21, heating the base oil, adding the boronized polyisobutylene bis-succinimide and the thiocarbamate, and stirring; s22, sequentially adding an antioxidant, an anti-wear agent, dodecenylsuccinic acid, DISUPER S24 and a metal deactivator into the solution obtained in the step S11, heating to 80 DEG C, and reacting for 2 hours; and S23, adding graphene nanosheets into the solution obtained in the step S22, and carrying out ultrasonic dispersion for 1 hour to obtain the product.

The invention discloses a functional hydrogel microsphere and a preparation method and application thereof, and relates to the technical field of medicines.The preparation method comprises the steps that a hyaluronic acid methacrylic acid precursor solution and an IL-1beta shRNA adenovirus stock solution are mixed to obtain an Ad-atHAMA precursor solution; preparing the Ad (at) HAMA precursor solution through an oil-in-water micro-fluidic technology to obtain an Ad (at) HAMA microsphere; and sequentially adding the Ad (at) HAMA microspheres, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide and N-hydroxysuccinimide into a 2-morpholinoethanesulfonic acid buffer solution, carrying out activating treatment, adding E selectin, and incubating to obtain the functionalized hydrogel microspheres. The functionalized hydrogel microspheres can inhibit a related mechanism of acute spinal cord injury pathological progress and promote neural function repair by targeting adsorption of neutrophil to regulate Nets-triggered innate immune inflammation cascade.

The invention discloses a preparation method of deuterated methylamine hydrochloride and a solid-phase continuous flow synthesis system, and relates to the technical field of deuterated synthesis. The preparation method comprises the following steps: adding out-of-phase polykadexide into methyl trifluoromethanesulfonate and 1, 2-dichloroethane for heating reaction, then adding methanol for quenching reaction, washing and drying to obtain an out-of-phase polykadexide type methyl reagent; the method comprises the following steps: adding a heterophase polysulfide-type methyl reagent into a mixed solvent of a polar solvent and heavy water, and carrying out alkali treatment to complete deuteration conversion, so as to obtain a heterophase polysulfide-type deuterated methyl reagent; the preparation method comprises the following steps: dissolving o-phenylsuccinimide in acetonitrile, and adding a heterophase polysulfide deuterium methyl reagent and inorganic alkali to react, so as to obtain N-(1, 1, 1-trideuterium methyl) benzo-succinimide; the preparation method comprises the following steps: hydrolyzing N-(1, 1, 1-trideuterium methyl) benzo-succinimide and hydrochloric acid in an aqueous solvent to obtain deuterated methylamine hydrochloride. The preparation method is simple, the deuterium source is cheap, the atom utilization rate is high, the deuteration rate is high, and the production cost is low.

The invention discloses a preparation method of alpha-chloro-4-methylsulfonyl acetophenone. The preparation method comprises the following steps: step A, reacting a compound as shown in a formula I with trimethyl orthoformate and N-chlorosuccinimide in an organic solvent to obtain a compound as shown in a formula II; and B, reacting the compound shown in the formula II with a sulfuric acid aqueous solution in an organic solvent to obtain a compound shown in a formula III. The chlorination method provided by the invention has the advantages of high yield, no generation of dichloro impurity and high product purity, and can be used as a rofecoxib or imrecoxib intermediate; the method is simple to operate, mild and controllable in reaction condition, capable of being amplified to kilogram-level reaction and suitable for industrial production.

The invention discloses a compound and a preparation method thereof, a hole transport material and a perovskite solar cell, and belongs to the technical field of materials. The structure of the compound is as follows: # imgabs0 # 10lt; nlt; 10000, and n is an integer; and Ar is an aniline fluorene group or a diphenylamine group. The preparation method comprises the following steps: reacting dithienopyrrole, 4-bromobenzaldehyde and a catalyst I to obtain an intermediate I; reacting the intermediate I with bromo-succinimide to obtain an intermediate II; reacting the intermediate II, aniline fluorene or diphenylamine substances and a catalyst II to obtain an intermediate III; reacting the intermediate III with sodium borohydride to obtain an intermediate IV; reacting the intermediate IV with acryloyl chloride to obtain an intermediate V; mixing and reacting the intermediate V and an initiator to obtain the compound. As a hole transport material, the compound is relatively high in decomposition temperature, high in stability, good in film-forming property and good in mobility, and is beneficial to the photoelectric conversion effect of a perovskite solar cell.

The invention belongs to the technical field of synthesis of ester compounds, and particularly relates to a preparation method of 2, 6-dichloro-4-cyanobenzoic acid methyl ester, which comprises the following steps: by taking dimethyl 2-aminoterephthalate as a raw material, sequentially carrying out substitution reaction, deamination reaction, hydrolysis reaction, amidation reaction and dehydration reaction to obtain the 2, 6-dichloro-4-cyanobenzoic acid methyl ester. The 2, 6-dichloro-4-cyanobenzoic acid methyl ester is prepared by the method, and the yield reaches 59.28%. The N-chlorosuccinimide is used as a chlorine source to carry out substitution reaction on the 2-amino dimethyl terephthalate, so that the potential safety hazard caused by the traditional chlorination reagent is avoided, and the tert-butyl nitrite used in the deamination reaction avoids the potential safety hazard caused by the use of strong corrosive sulfuric acid; the amidation reaction is completed in one step by adopting a condensing agent, so that the complicated operation caused by firstly preparing acyl chloride and then carrying out condensation reaction is avoided, and therefore, the preparation method has the characteristics of safe preparation process, environment friendliness, simplicity in operation and the like under the condition of ensuring the product yield and purity.

The invention relates to a method for synthesizing an iodo-pyridine compound from N-propargyl enaminone, which comprises the following steps: by taking N-propargyl enaminone as a raw material, DMF (Dimethyl Formamide) as a reaction solvent and copper acetate and N-iodosuccinimide as accelerators, carrying out intramolecular coupling reaction at 60 DEG C to synthesize the iodo-pyridine compound. The method for directly synthesizing the pyridine heterocyclic compound through the intramolecular coupling reaction of the N-propargyl enaminone under the non-alkaline condition is disclosed for the first time, reaction substrates are not limited to benzene rings on alkynyl, the application range of the reaction is greatly expanded, and the method has the advantages of being wide in substrate range, strong in functional group application range, mild in reaction condition, easy to operate, safe, high in yield and the like. And raw materials are cheap.

The invention provides a synthetic method of a bromo-pyrazole intermediate for preparing loratinib, which comprises the following steps: 1, adding a solvent and a compound 19 into a reaction kettle, and then adding a bromination reagent N-bromo-succinimide in batches to synthesize a compound 14; 2, adding dichloromethane, the compound 14 and triethylamine into a reaction kettle, and then dropwise adding trifluoroacetic anhydride to synthesize a compound 15, namely the key intermediate bromo-pyrazole of the loratinib; according to the synthetic method of the bromo-pyrazole intermediate for preparing the loratinib, the adopted starting materials are low in price, the route is simple, the yield is high, the purity is good, the cost is reduced by 40% or above compared with an existing synthetic route, the production cost can be greatly reduced, and the industrial competitiveness is improved.

The application relates to the technical field of organic synthesis, and discloses a synthesis method of a benzoyl modified nucleoside, which comprises the following steps: dissolving or suspending a substrate in a solvent, adding N-chlorosuccinimide, reacting at a certain temperature, generating a corresponding N-chloroamine intermediate, then adding a certain equivalent of benzaldehyde, and generating a final product under the joint action of an oxidant and a catalyst. According to the method, the hydroxyl group on the sugar ring does not need to be protected, and is directly reacted with the amino group on the base, so that the side reaction is less, the obtained product is high in purity, and the yield is high.

The present invention belongs to the technical field of lithium-ion battery slurries, and specifically relates to a lithium-ion battery aqueous positive electrode slurry and a preparation method thereof. The components include 50-60 parts of positive electrode active material, 6-10 parts of carbon nanotube dispersion, 1-5 parts of conductive agent, 1-3 parts of aqueous binder, and 40-50 parts of deionized water. In the present invention, deionized water is used as a solvent to increase the fluidity of carbon nanotubes (CNTs), reduce the viscosity of CNTs, and reduce environmental pollution. Then, a certain proportion of polyisobutenyl succinimide and α-olefin sulfonate are added to improve the dispersion stability of CNTs, reduce the fluidity of the slurry, increase the friction coefficient of the dispersion axis, and prevent CNTs from adhering to the binder and forming agglomerates. The prepared lithium-ion battery aqueous positive electrode slurry has good consistency, high stability, and is not prone to sedimentation.

This invention belongs to the field of coolant technology, specifically relating to a coolant and its application in an immersion liquid-cooled energy storage system. The coolant, by weight, comprises 80-95 parts base oil, 1-5 parts thermally conductive nanoparticles, 0.5-2 parts composite dispersant, 0.3-1 part composite corrosion inhibitor, 0.1-0.5 parts antioxidant, 0.2-0.5 parts pour point depressant, and 0.01-0.05 parts defoamer. The base oil is a mixture of polyalphaolefin and synthetic ester, and the composite dispersant is a compound of polyisobutylene succinimide and Mannich base dispersant. Aging tests show that this coolant exhibits high thermal conductivity retention, low acid value increase, and low corrosion rate. The coolant of this invention can effectively maintain the dispersion stability of nanoparticles in the environment of precipitates from sealing materials, extending the fluid change cycle.

The application belongs to the technical field of biological medicine, and discloses a synthesis method of aryl F-18 labeled sulfuryl chloride and application of the aryl F-18 labeled sulfuryl chloride in amine compound labeling. The method takes thiophenol derivative as a labeling precursor, obtains F-18 labeled thiophenol intermediate through photocatalytic aryl F-18 fluorination reaction, and then obtains aryl F-18 labeled sulfuryl chloride through N-chlorosuccinimide oxidation chlorination. The obtained aryl F-18 labeled sulfuryl chloride (4-[ 18 F] fluorobenzenesulfonyl chloride) can occur sulfurylization reaction with various amine compounds at room temperature, and the radiochemical conversion rate is as high as 98%. The application is successfully applied to novel synthesis of AMPA receptor PET imaging agent[ 18 F]2 (the conversion rate is 96%, which is much higher than 13% reported in the literature). The application has the advantages of mild reaction condition, high conversion rate and wide substrate application range, and provides an efficient method for innovative preparation of F-18 labeled PET probes.

The invention belongs to the field of Velciguat synthesis, and particularly relates to a preparation method of Velciguat and an intermediate product thereof. The preparation method of the Velciguat comprises the following steps: (1) reacting aminomalononitrile with methyl chloroformate to generate an intermediate product I; (2) carrying out ring closing on the intermediate product I and formamidine under an alkaline condition to obtain an intermediate product II; (3) carrying out bromination reaction on the intermediate product II and N-bromosuccinimide to obtain an intermediate product III; (4) reacting the intermediate product III with bis (pinacolato) diboron under the action of a catalyst to obtain an intermediate product IV; and (5) carrying out a reaction on the intermediate product IV and 5-fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo [3, 4-b] pyridine to prepare the viriciguat. The method is simple to operate, low in cost and safe in production. The invention also provides the intermediate product obtained by the preparation method.

The invention discloses a lubricating oil additive composition. The lubricating oil additive composition is prepared from the following components in percentage by mass: 10 to 30 weight percent of zinc dialkyl dithiophosphate, 10 to 30 weight percent of succinimide dispersing agent, 15 to 40 weight percent of metal clearing agent and 5 to 10 weight percent of dialkyl dithiophosphate acrylate anti-wear agent, 10-20 wt% of an alkyl biimidazole phosphate ionic liquid, and 5-10 wt% of an alkylated diphenylamine antioxidant. The alkyl bis-imidazole phosphate ionic liquid and the propylene tetrapolymer alkylated diphenylamine are compounded, so that the lubricating oil has excellent oxidation resistance and corrosion inhibition performance in mineral oil and synthetic oil, can reduce the friction coefficient of oil products, and is suitable for vehicle transmission oil, vehicle drive axles or electric transmissions, and the like. And the service condition requirement of long service life of a vehicle transmission system is met.

The invention discloses a preparation method of 3-chloro-2,4,5-trifluorobenzoic acid and application thereof, comprising the following steps: S1: adding bromine dropwise to 1,2,4-trifluorobenzene at 10-30°C to carry out bromination reaction; S2: adding N-chlorosuccinimide in batches to the obtained 2,4,5-trifluorobromobenzene and concentrated sulfuric acid at 5-10°C to carry out substitution reaction and purification; S3: adding magnesium chips and tetrahydrofuran to an anhydrous reaction bottle, adding the obtained 3-chloro-2,4,5-trifluorobromobenzene under stirring, heating to 35-40°C to initiate reaction, then adding bromobenzene dropwise, keeping warm and stirring for reaction for 1h, then cooling to 5-10°C, adding dry ice in batches to carry out Grignard reaction, adding ultrapure water when the system is no longer exothermic, adjusting pH=1, filtering by suction and drying; and S4: recrystallization. The invention uses 1,2,4-trifluorobenzene as a raw material, and obtains a target product through bromination, chlorination, Grignard reaction and recrystallization. The reaction process is simplified, the operation is simple, the reaction is mild, the product yield is more than 90%, the purity is more than 99.9%, the by-products in the reaction process are few, and the production cost is low.

The invention discloses a diesel engine lubricating oil composition and a preparation method thereof, and the diesel engine lubricating oil composition comprises the following components by mass: 5.0%-7.5% of a high temperature detergent, 2.5%-5.4% of a bis-succinimide dispersant, 0.5%-2.0% of a zinc dialkyl dithiophosphate antioxidant preservative, 0.5%-1.5% of an auxiliary antioxidant, 0.5%-1.5% of a 2, 3-dihydro-2, 3, 4-trimethyl-1, 3-pentanediol monoisobutyrate, 0.5%-1.5% of a 2, 3, 4-trimethyl-1, 3-pentanediol monoisobutyrate, 0.5 The lubricating oil composition is prepared by uniformly stirring the following components in percentage by weight: 0.5 to 2.0 percent of 2, 2-dimethyl-7-benzofuryl-A-N-carbamate, 0.2 to 0.5 percent of pour point depressant, 0.0015 to 0.0050 percent of methyl silicone oil anti-foaming agent and the balance of catalytic hydrogenation base oil at the temperature of between 60 and 70 DEG C. The lubricating oil composition can be prepared by uniformly stirring the components at the temperature of between 60 and 70 DEG C. According to the diesel engine oil composition, various components are reasonably compounded, so that mutual inhibition of marine diesel engine oil water separation property, additive washing resistance, detergency and dispersibility, oxidation resistance, wear resistance and the like is solved, and the oil change period of an oil product is greatly prolonged.

The invention relates to a copper-tin alloy electroplating solution for barrel plating. The copper-tin alloy electroplating solution for barrel plating comprises the following components in parts by mass: 80 g / L to 120 g / L of hydrochloric acid, 15 g / L to 25 g / L of copper chloride, 10 g / L to 30 g / L of stannous chloride, 15 g / L to 25 g / L of stannous pyrophosphate, 15 g / L to 35 g / L of copper pyrophosphate, 5 g / L to 10 g / L of sodium chloride, 20 g / L to 40 g / L of succinimide, 0.01 g / L to 0.02 g / L of sodium citrate, 40 g / L to 60 g / L of a complexing agent, 0.2 g / L to 0.6 g / L of a brightening agent, 4 g / L to 8 g / L of a dispersing agent, 0.1 g / L to 0.2 g / L of a stabilizing agent and 30 g / L to 50 g / L of a buffering The copper-tin alloy electroplating solution for barrel plating is a cyanide-free electroplating solution, and the influence on the environment is greatly reduced in the production process. The copper-tin alloy electroplating solution for barrel plating can form a compact plating layer on a plating piece, and the bonding performance of the plating layer and the plating piece is stable, so that a protective layer with corrosion resistance and friction resistance is formed on the surface of the plating piece.

The invention relates to the technical field of compound synthesis, in particular to a method for directly reducing carboxylic acid into aldehyde. The preparation method comprises the following steps: mixing triphenylphosphine, dichloromethane, carboxylic acid and N-chlorosuccinimide, and reacting to obtain a reactant; mixing with pinacol borane and 4-dimethyl pyridine, and continuously reacting to obtain a continuous reactant; and separating and purifying to obtain aldehyde. The synthesis of the substrate carboxylic acid provided by the invention and the rapid deoxidation of the carboxylic acid are carried out to obtain an aldehyde product, especially the following compounds 2aa, 2ab, 2ae, 2bc, 2be, 2bf, 2bg, 2bh, 2bi, 2bj, 2bk and 2bl have catalytic hydrolysis effects on hypophosphamide; the compound 2bl has a particularly excellent effect on hydrolysis of hypophosphamide.

The present invention relates to the technical field of detection systems, in particular to a system for detecting the content of N-bromosuccinimide in sodium sugammadex. The system comprises a chromatograph main body for elution and separation and a mass spectrometer main body for detection, wherein a column oven is connected between the chromatograph main body and the mass spectrometer main body, and a chromatographic column for sample elution and separation is assembled in the column oven; a liquid inlet seat and a liquid outlet seat are provided in the column oven, respectively communicating with the chromatograph main body and the mass spectrometer main body, and the chromatographic column is positioned and assembled between the liquid inlet seat and the liquid outlet seat; a telescopic joint structure is provided at the end of the chromatographic column, the chromatographic column is connected to the liquid inlet seat and the liquid outlet seat via the joint structure, and a glass wool column can be positioned and loaded in the joint structure; a combined water bath structure is provided in the column oven based on an inner partition, and the assembled water bath structure can seal the chromatographic column main body structure; the present invention can achieve the purpose of improving the accuracy of content detection.

The invention belongs to the technical field of deuterated organic chemical synthesis, and particularly relates to a synthesis method of deuterated 9-phenyl anthraceneboronic acid-D8, which comprises the following steps of: 1, halogenation reaction: reacting 9-phenyl anthracene-D9, bromo-succinimide (NBS) and triethylamine (TEA) in dichloromethane at low temperature to generate an intermediate 9-phenyl-10-bromoanthracene-D8; step 2, carrying out nucleophilic reaction of forming carbon negative by pulling out bromine with strong in a low-temperature environment of-65 DEG C to-70 DEG C, reacting n-butyllithium with the intermediate 9-phenyl-10-bromoanthracene-D8 in 2-methyltetrahydrofuran to generate 9-phenyl anthracene lithium; then triisopropyl borate is added for a boronation reaction, and the 9-phenyl anthracene boric acid-D8 is obtained after hydrochloric acid hydrolysis and purification. The purity of the deuterated 9-phenyl anthracene boric acid-D8 is greater than or equal to 99.8%, the deuteration rate is greater than or equal to 98%, and the deuterated 9-phenyl anthracene boric acid-D8 is suitable for being used as

The present invention discloses a method for preparing N-hydroxysuccinimide. The method uses a weakly acidic cation exchange resin as a catalyst. By reducing the acidity of the reaction system, product decomposition can be avoided, thereby improving product yield and quality. The method also reduces the reaction temperature, lowers equipment anti-corrosion requirements, extends equipment service life, reduces energy consumption, and is more conducive to industrial implementation. Furthermore, the catalyst is recyclable and does not require the addition of a stabilizer, making it more environmentally friendly.

The method for manufacturing an intermediate compound for shikonin synthesis of the present invention comprises the steps of: reacting 1,5-dihydroxynaphthalene with dimethyl sulfate to prepare 1,5-dimethoxynaphthalene; reacting 1,5-dimethoxynaphthalene with N-bromosuccinimide (NBS) to prepare 1,5-dibromo -4,8-dimethoxynaphthalene; introducing a methoxy group into 1,5-dibromo-4,8-dimethoxynaphthalene using copper iodide (CuI) and 1,10-phenanthroline as a catalyst to prepare 1,4,5,8-tetramethoxynaphthalene; performing formylation of 1,4,5,8-tetramethoxynaphthalene using phosphoryl chloride (POCl3) to prepare 2-formyl-1,4,5,8-tetramethoxynaphthalene; and forming a boron complex using pinacolborane (HBpin) and 3,3-dimethylallyl bromide and reacting the boron complex with 2-formyl -1,4,5,8-tetramethoxynaphthalene to prepare a prenylated shikonin intermediate. Compared to conventional synthetic methods, the method of the present invention offers milder reaction conditions, shorter reaction time, and improved yield, thereby greatly enhancing the economic feasibility of shikonin synthesis.

The application belongs to the technical field of organic synthesis, and provides a star structure carbazole derivative, a preparation method thereof and a carbazole conductive polymer. The application obtains an intermediate by mixing 10-phenyl-10H-phenothiazine, N-bromosuccinimide and a first organic solvent for reaction; obtains the star structure carbazole derivative by mixing the intermediate, 9H-carbazole-2-boronic acid pinacol ester, tetrakis(triphenylphosphine)palladium, an accelerator and a second organic solvent for reaction; and obtains the carbazole conductive polymer by mixing the star structure carbazole derivative and an electrolyte solution for cyclic voltammetry electrochemical polymerization. The method is simple, has few by-products, and the star structure carbazole derivative obtained by the method is a non-coplanar star structure, which is beneficial to the embedding and discharging of electrolyte ions, so that the carbazole conductive polymer has excellent electrochemical performance and energy storage properties, and the conductive polymer also has excellent electrochromic performance.

The invention discloses a preparation process of 5-bromonicotinic acid, which comprises the following steps: sequentially adding ethyl nicotinate and pinacol borane into a reaction kettle, heating to react, adding N-bromosuccinimide into the reaction kettle, maintaining the reaction temperature, and filtering to remove a byproduct succinimide after the reaction is finished. And carrying out reduced pressure distillation to recover the solvent to obtain the ethyl 5-bromonicotinate. Adding ethyl 5-bromonicotinate into another reaction kettle, adding an alkali solution, heating, stirring for reaction, cooling reaction liquid after the reaction is finished, dropwise adding hydrochloric acid to adjust the pH value, cooling, crystallizing, filtering, washing a filter cake, and drying to obtain a 5-bromonicotinic acid finished product. The total yield gt of the preparation process of the 5-bromonicotinic acid; the HPLC purity is gt; 99%. The process is simple and convenient to operate and easy to implement, raw materials are cheap and easy to obtain, reaction conditions are mild, high-temperature and high-pressure reaction is not needed, and requirements on equipment are reduced. The whole process is safer to the environment, and green and pollution-free production can be realized.

This invention discloses a two-photon fluorescent dye, prepared as follows: 6-hydroxy-2-naphthaldehyde reacts with a dihaloalkane under alkaline conditions to obtain a monohaloalkane-based aryl ether, which is then reacted with an aqueous trimethylamine solution to prepare S1; diethyl 4-(4-tolyl)pyridine-2,6-dicarboxylate reacts with N-bromosuccinimide to obtain a brominated product, which is then reacted with triphenylphosphine to prepare S2. After intermediates S1 and S2 react under strongly alkaline conditions, the product is then hydrolyzed to prepare the target product. This dye exhibits good cell membrane permeability, good dispersion in the cytoplasm, preferentially targets organelles in the cytoplasm, is water-soluble, has very low toxicity, and a high two-photon absorption interface, making it suitable for two-photon fluorescence confocal microscopy imaging.