36 results about "Cyanoacetic acid" patented technology

The invention belongs to the technical field of fine chemical engineering, and discloses a synthesis method of a malonate compound, which comprises the following steps: under the action of a heterogeneous catalyst, carrying out hydrolysis-esterification reaction on cyanoacetic acid and alcohol, and after the reaction is finished, carrying out post-treatment to obtain the malonate compound, the heterogeneous catalyst comprises a carrier and an active component; the active component comprises ionic liquid and active metal; the carrier is an ordered mesoporous material; the active metal is alkaline earth metal. According to the method, malonate products can be obtained, the problems of low yield, serious equipment corrosion and large amount of three wastes are solved, efficient synthesis of malonate compounds is realized, meanwhile, the production efficiency is improved, and the environmental pollution is greatly reduced.

The application discloses a catalyst for preparing malononitrile, a preparation method of the catalyst and a method for preparing malononitrile by using the catalyst. The catalyst is a solid catalyst, which is an acidic catalyst loaded with rare earth metal oxide. The method for preparing malononitrile is that cyanoacetic acid or cyanoacetate or cyanoacetamide and an ammonia source are subjected to ammoniation dehydration reaction in a continuous reactor to prepare malononitrile according to a certain molar ratio. Then, vacuum distillation (20 torr-25 torr) is carried out, and a fraction collected at 110 DEG C-120 DEG C is malononitrile product. The ammonia source can be ammonia gas, ammonia water, ammonium carbonate or urea. The method for preparing malononitrile can reduce production cost, improve production safety, reduce the discharge amount of three wastes in the preparation of malononitrile by using an existing process, and improve product quality, and is a sustainable and green synthesis route.

This invention relates to the field of solid propellant technology, specifically disclosing a neutral polymer bonding agent, its preparation method, and its application in solid propellants. The neutral polymer bonding agent is prepared by polymerization of poly(hydroxyalkyl polyacrylate) and cyanoacetic acid as raw materials. It can achieve controllable molecular weight and controllable proportion of functional groups in the polymer. Moreover, the active group -CN in the neutral polymer bonding agent has low steric hindrance and is more easily adsorbed on the surface of ammonium nitrate particles, thereby improving the bonding effect.

The invention discloses an environment-friendly phenol-free thermo-sensitive paper label material and a preparation method thereof, and relates to the technical field of thermo-sensitive paper. When the environment-friendly phenol-free thermo-sensitive paper label material is prepared, cellulose sequentially reacts with cyanoacetic acid, 4-(2-chloroethyoxyl) benzophenone and N, N-dimethylpropyl-1-amine to prepare modified cellulose; the preparation method comprises the following steps: carrying out reaction on silicon dioxide and diethylenetriamine propyl trimethoxy silane to prepare pre-modified silicon dioxide; reacting the pre-modified silicon dioxide, phosphorous acid and formaldehyde to obtain modified silicon dioxide; uniformly mixing functional styrene-butadiene emulsion, modified cellulose, modified silicon dioxide, a color developing agent, a lubricating agent, a sensitizer and colorless pigment to prepare a thermosensitive coating; and uniformly coating the surface of thermosensitive base paper with the thermosensitive coating by using a coating machine, and drying to obtain the environment-friendly phenol-free thermosensitive paper label material. The environment-friendly phenol-free thermo-sensitive paper label material prepared by the invention has excellent wear resistance, antibacterial property, light resistance and flame retardance.

The present invention relates to a catalyst and a preparation method thereof. The catalyst comprises a mesoporous γ-Al2O3 / SiO2 support and an active component supported on the support. The active component is a complex formed by a metal salt and a modifier. The modifier is a reaction product of a first component selected from organic acids and / or inorganic acids and a second component selected from organic bases. The catalyst is weakly acidic. The present invention also relates to a method for synthesizing malonic ester compounds, comprising: mixing cyanoacetic acid, water and the catalyst and performing an activation treatment, then carrying out a hydrolysis reaction on the first mixed material obtained by the activation treatment in the presence of a catalyst for cyanoacetic acid hydrolysis reaction, and then adding an alcohol to the second mixed material obtained by the hydrolysis reaction to carry out an esterification reaction to obtain malonic ester compounds. The catalyst of the present invention can effectively solve problems such as low yield, serious equipment corrosion, and large amounts of "three wastes", and environmentally friendly and efficiently realizes the synthesis of malonic ester compounds.

The present invention belongs to the technical field of solar energy industry, and specifically relates to a hole transport material containing halogen and its application as an organic hole transport material. The present invention designs a cyanoacetic acid or cyanophosphoric acid as an anchoring group, and introduces halogen into the molecular structure through a self-assembled monolayer strategy, thereby obtaining a new type of hole transport material containing halogen, the purpose of which is to solve the technical problems such as poor stability and poor device performance faced by existing organic small molecule hole transport materials with anchoring groups. In addition, the present invention also relates to a perovskite battery and a flexible perovskite battery prepared using the aforementioned organic hole transport material. The beneficial effect of the present invention is that the introduction of halogen atoms in the material can improve the stability of the battery and extend its service life.

The present invention discloses an interface modification material, a fully printed carbon-based perovskite cell, and a preparation method thereof. The interface modification material preparation process is as follows: Br-NI is prepared using 4-bromo-1,8-naphthoic anhydride and 3-aminopentane as raw materials; a degassed mixture of THF and an aqueous potassium carbonate solution is added to a mixture of Br-NI, 5-(4,4,5,5-tetramethyl-1,3,2-dioxabicyclo-2-yl)thiophene-2-carboxaldehyde, and tetrakis(triphenylphosphine)palladium, and the mixture is stirred under an argon atmosphere for complete reaction, followed by post-processing to obtain CTNI; CTNI, cyanoacetic acid, and piperidine are mixed in anhydrous chloroform and stirred under an argon atmosphere for complete reaction, followed by post-processing to obtain a CATNI interface modification material. The present invention also discloses a carbon-based perovskite solar cell, which comprises, from bottom to top, a conductive substrate, an electron transport layer, an interface modification layer, a perovskite layer, a hole transport layer, and a carbon electrode. The present invention significantly improves the voltage and efficiency of the device through modification of the interface modification layer, thereby improving the performance of the perovskite cell.

The invention provides a synthesis method of L-3-aminoisobutyric acid. The synthesis method comprises the following steps: enabling a dichloromethane solution of cyanoacetic acid to react with oxalyl chloride; a reaction product, (S)-4-benzyl-2-oxazolidinone dissolved in dichloromethane and triethylamine are respectively fed into a continuous flow reactor to be mixed and react with the (S)-4-benzyl-2-oxazolidinone dissolved in dichloromethane; collecting reaction liquid, extracting, concentrating and recrystallizing to obtain a compound 2; dissolving the compound 2 in tetrahydrofuran, and adding iodomethane; respectively feeding the mixed solution and a tetrahydrofuran solution of lithium diisopropylamide into a continuous flow reactor for mixing reaction; collecting reaction liquid, quenching and purifying to obtain a compound 3; dissolving the compound 3 in a mixed solvent of an organic solvent and water, adding lithium hydroxide and hydrogen peroxide, and reacting; adding a sodium sulfite aqueous solution for quenching reaction, extracting, concentrating and purifying to obtain a compound 4; dissolving a compound 4 in ethanol, and carrying out a continuous flow hydrogenation reaction with hydrogen through a continuous flow hydrogenation reactor; and collecting a reaction product, concentrating, cooling and crystallizing to obtain the L-3-aminoisobutyric acid.

The invention relates to the technical field of high polymer materials, in particular to modified hydrogenated butadiene-acrylonitrile rubber with high cyano content as well as a preparation method and application of the modified hydrogenated butadiene-acrylonitrile rubber. The modified hydrogenated butadiene-acrylonitrile rubber contains a cyanoacetate side chain segment, and the molar content of cyano groups in the modified hydrogenated butadiene-acrylonitrile rubber is greater than or equal to 40%. According to the modified hydrogenated nitrile rubber with the high cyano content, a cyanoacetate side chain is introduced through the ring-opening reaction of the epoxidized hydrogenated nitrile rubber and cyanoacetic acid, the novel hydrogenated nitrile rubber is prepared, the cyano content can be regulated and controlled by controlling the acrylonitrile content and the epoxidation degree of original rubber, the cyano content can reach 56%, and the cyano content can reach 50%. And the material can be endowed with excellent oil resistance.

The application provides a continuous production device and method of methyl cyanoacetate, which comprises a feeding unit, a reaction unit and a post-treatment unit connected in sequence, the reaction unit comprises a tubular reactor, the lower part of the tubular reactor is provided with a methanol feeding port and a sodium cyanide feeding port, the top of the tubular reactor is provided with a methyl chloroacetate feeding port, and the bottom of the tubular reactor is provided with a methyl cyanoacetate crude product discharging port; the feeding unit comprises a methanol feeding device, a sodium cyanide feeding device and a methyl chloroacetate feeding device, and the methanol feeding device, the sodium cyanide feeding device and the methyl chloroacetate feeding device are connected with the methanol feeding port, the sodium cyanide feeding port and the methyl chloroacetate feeding port respectively. The tubular reactor is used for continuous production, compared with the traditional batch production mode of the reaction kettle, the problem of sodium cyanide solid feeding is solved, the occurrence of the reverse reaction is effectively inhibited, and the yield of methyl cyanoacetate is greatly improved.

The utility model relates to the technical field of dehydration, and discloses a novel cyanoacetic acid dehydration device which comprises an incoming material input pump, the incoming material input pump is connected with a preheating mechanism through a pipeline, the preheating mechanism comprises a water storage tank, an electrical bar, a flow guide pipe, a spherical shell and heat collection fins, the electrical bar is installed in the water storage tank, the flow guide pipe is installed in the water storage tank, and the spherical shell is installed in the spherical shell. The left end of the flow guide pipe is connected with the incoming material input pump through a pipeline, the right end of the flow guide pipe is connected with an inlet of the horizontal film evaporator through a pipeline, a plurality of spherical shells are arranged on the flow guide pipe, a steam outlet is formed in the upper right portion of the horizontal film evaporator, and a concentrated solution outlet is formed in the lower right portion of the horizontal film evaporator. The steam outlet is connected with an inlet of the first-stage condenser through a pipeline, and an outlet of the first-stage condenser is connected with an inlet of the second-stage condenser through a pipeline. According to the cyanoacetic acid dehydration device, cyanoacetic acid is preheated firstly, and then the film evaporator is used for rapidly dehydrating the cyanoacetic acid, so that moisture in the cyanoacetic acid is conveniently, rapidly and fully removed.

The invention relates to a preparation method of 7-methoxynaphthalene acetonitrile. The preparation method comprises the following steps: reacting 7-methoxy-1-tetralone with copper bromide under the action of a catalyst to generate 7-methoxy-2-bromo-1,2,3,4-tetralone; reacting 7-methoxy-2-bromo-1,2,3,4-tetralone under the catalysis of a heteropoly acid to obtain 7-methoxy-1,4-dihydronaphthalone; and directly condensing 7-methoxy-1,4-dihydronaphthalone with cyanoacetic acid in the presence of benzylamine and heptanoic acid to obtain 7-methoxynaphthalene acetonitrile. The preparation method of the catalyst comprises the following steps: mixing carrier particles and a metal salt solution, adjusting the pH to alkaline, washing, drying, immersing in a sulfuric acid solution, filtering, and then roasting to obtain the catalyst. The carrier particles are aluminum oxide or silicon dioxide, and the metal salt solution is a salt solution of Zr, Ti or Sn. The method reduces the difficulty of purification, improves the yield and purity, and reduces the cost.

The invention relates to a ternary lithium battery electrolyte and a preparation method and application thereof, and belongs to the technical field of lithium battery materials. By synthesizing the ester compound with sulfonate, cyanoacetate and a phosphorus-containing branched structure, the comprehensive performance of the electrolyte can be effectively improved, the branched structure is beneficial to reducing the viscosity of the electrolyte, and the ester bond is beneficial to improving the compatibility of the additive and an electrolyte system, so that the proton motion resistance is reduced, the activation energy of ion migration is reduced, and the service life of the electrolyte is prolonged. And sulfonate, cyanoacetate and phosphorus atom centers can further improve the conductivity of the electrolyte. The ternary lithium battery electrolyte provided by the invention has good conductivity in both room-temperature and low-temperature environments, and provides a good basis for the use of a lithium battery in the low-temperature environment.

The invention discloses a tire polish and a preparation method thereof, and relates to the technical field of polishes. When preparing the tire polish, the present invention first reacts a polyurethane terminated with methyl ethyl ketoxime with diaminothiourea, then reacts with 3-thiophenecarbonyl chloride, and then polymerizes with thiophene to obtain a modified polyurethane; secondly, 3-aminopropyl polydimethylsiloxane is reacted with carbon disulfide and phosphorus oxychloride, then reacts with 4-aminobenzophenone, and finally reacts with methyl cyanoacetate to obtain a modified silicone oil; finally, a modified polyurethane emulsion, modified silicone oil, liquid wax, solvent oil, pure water, ethylene glycol, methylcellulose, and sodium dodecylbenzenesulfonate are reacted. The tire polish prepared by the present invention has good antibacterial and antistatic properties.

The application discloses a modified lithium-rich manganese-based positive electrode material and a preparation method and application thereof, and belongs to the technical field of positive electrode materials. The preparation method comprises the following steps: (1) adding an acid with high electronegativity into a solvent to obtain an acid solution; adding a MOF material into the acid solution, heating and reacting for a set time, and then performing solid-liquid separation to obtain a MOF material containing a high-electronegativity anion group; wherein the acid with high electronegativity is one or more of trifluoromethanesulfonic acid, trinitrobenzenesulfonic acid and cyanoacetic acid; (2) mixing the MOF material containing the high-electronegativity anion group with a lithium-rich manganese-based positive electrode material in a solid phase to obtain a modified lithium-rich manganese-based positive electrode material. In the application, the MOF material is treated by the acid with high electronegativity and then is compounded with the lithium-rich manganese-based positive electrode material, so that the ion transmission rate of the interface of the positive electrode material can be effectively improved, the polarization phenomenon of the positive electrode material can be reduced, and the rate performance of the material can be improved.

The application discloses a kind of double carbazole compounds and its preparation method and co-sensitization application, specific preparation process is compound shown in formula II-1, formula II-2, formula II-3, formula II-4 or formula II-5 and cyanacetic acid are dissolved in solvent, basic substance is added, heated reflux reaction under stirring, after reaction, reaction liquid is concentrated to remove solvent, the obtained concentrate is dissolved in eluent and separated and purified by column chromatography silica gel, eluent is collected and eluent is evaporated, i.e. the target product such as compound of formula DSB-1, formula DSB-2, formula DSB-3, formula DSB-4 or formula DSB-5 is prepared, and it is used for preparing dye sensitization agent, the application is connected by alkyl chain double carbazole, and benzothiadiazole acceptor and aromatic heterocycle are introduced in a carbazole, another carbazole is introduced as bridge bond, cyanacetic acid is used as acceptor, double carbazole compound is synthesized, and new applicable material is added for the screening of dye sensitization agent.

The invention discloses a preparation method of fluopyram, which comprises the following steps: mixing 2, 3-dichloro-5-trifluoromethylpyridine, a solvent and alkali, dropwise adding cyanoacetate for reaction, adding an N-acetoxymethyl-2-trifluoromethyl benzamide solution for reaction, adding methanol, a sodium hydroxide solution and a hydrogen peroxide solution for catalytic hydrolysis, adding a sodium hydroxide solution and a hydrogen peroxide solution for reaction, and performing reduced pressure distillation to obtain the fluopyram. And performing hydrochloric acid acidification and decarboxylation on the catalytic hydrolysis product to obtain the fluopyram. According to the preparation method of the fluopyram, the 2, 3-dichloro-5-trifluoromethylpyridine, the cyanoacetate and the N-acetoxymethyl-2-trifluoromethyl benzamide are taken as raw materials, and under the action of the hydrogen peroxide, not only can the preparation efficiency be improved, but also the fluopyram with high yield and high purity can be prepared; the method has the advantages of simple process, low cost, high preparation efficiency, high product yield, high purity, environmental protection and the like, can improve the product competitiveness, and is convenient for realizing industrial application.

The invention relates to the technical field of optoelectronic devices, in particular to a perovskite thin film, a preparation method thereof and a flexible perovskite solar cell. The perovskite thin film comprises a perovskite material layer and an SAM polymer film layer anchored on the surface of the perovskite material layer, the SAM polymer film layer comprises an SAM polymer, the SAM polymer comprises a plurality of SAM monomers which can be self-assembled and polymerized to form a film, and each SAM monomer comprises a terminal group and an anchoring group; the terminal group comprises at least one of carbazole, dibenzocarbazole and acridine; the anchor group includes at least one of phosphoric acid, carboxylic acid, boric acid, and cyanoacetic acid. According to the perovskite thin film, the SAM polymer is adopted as an additive or a passivator to modify a perovskite interface, holes can be effectively transmitted, a part of external force is counteracted as a perovskite protection layer, and the bending resistance of perovskite is improved; the method is suitable for flexible perovskite solar cells, and the anti-bending performance and efficiency are improved.

The invention relates to the technical field of organic synthesis, and particularly discloses a preparation method of octocrylene. According to the method, efficient synthesis of esterification and condensation cascade reaction is realized by adopting a one-pot method, cyanoacetic acid and isooctanol are subjected to esterification reaction in the presence of a bifunctional catalyst under the protection of inert gas, and then condensation reaction with benzophenone is carried out. Wherein the bifunctional catalyst is prepared by taking fluoro-triptycene trialdehyde as an organic framework porous structure and modifying a loaded metal active center in multiple steps, has high catalytic activity and stability, and improves the conversion rate and selectivity of the reaction.

The invention relates to the technical field of electrolytes, and provides a modified polymer solid electrolyte and a preparation method thereof. The modified polymer solid electrolyte is obtained by modifying a polymer electrolyte material mixed with lithium salt with ethyl acetate and triethylamine cyanoacetate, the raw materials of the polymer electrolyte material mixed with the lithium salt comprise a polymer electrolyte material and the lithium salt; the triethylamine cyanoacetate salt is prepared from the following raw materials: cyanoacetic acid and triethylamine; the ionic conductivity of the modified polymer solid electrolyte is more than 0.24 mS / cm, the lithium ion transference number is more than 0.32, and the tensile strength is more than 1.8 MPa. According to the technical scheme, the problems of poor ionic conductivity and poor structural stability of the polymer solid electrolyte in the prior art are solved.

The invention relates to a method for preparing (R)-4-((1-(2-cyanoacetyl) piperidine-3-yl) amino)-1H-pyrrolo [2, 3-b] pyridine-5-ethyl formate (compound 1). The process involves the addition of an ethyl formate group, the displacement of the halogen with a chiral amine, the deprotection of the chiral cyclic amine, and the subsequent coupling reaction with cyanoacetic acid. The displacement may be performed in an autoclave at elevated pressure.

The specific preparation process comprises the following steps: dissolving a compound as shown in a formula (II) and cyanoacetic acid or rhodanine-3-acetic acid in a solvent, adding an alkali catalyst, carrying out heating reflux reaction under stirring, and after the reaction is finished, concentrating to remove the solvent to obtain the bis (triphenylamine) benzothiadiazole compound as shown in the formula (II). The preparation method comprises the following steps: adding benzothiadiazole to two triphenylamine electron donors, dissolving the obtained concentrate in an eluent, carrying out separation and purification through column chromatography silica gel, collecting the eluent, and evaporating to remove the eluent so as to prepare a compound shown in the formula ZR-1 or ZR-4, and using the compound to prepare the dye sensitizer. The bistriphenylamine benzothiadiazole compound is synthesized by introducing an anchoring group and electron acceptor cyanoacetic acid or rhodanine-3-acetic acid on benzothiadiazole, so that a new applicable substance is added for screening of dye sensitizers, and the bistriphenylamine benzothiadiazole compound can be used for preparing the bistriphenylamine benzothiadiazole compound.

The invention relates to a preparation method of a medical adhesive, in particular to a preparation method of a high-yield alpha-cyanoacrylate medical adhesive, which can effectively improve the yield of alpha-cyanoacrylate on the premise of ensuring high purity. The preparation method comprises the following steps: under the combined action of a phase transfer catalyst and a hydrophobic inorganic nano-dispersant, carrying out condensation polymerization on cyanoacetate and formaldehyde to prepare a poly (alpha-cyanoacrylate) prepolymer, melting the prepolymer through a programmed temperature control process, heating to remove front fractions, rapidly heating to a depolymerization temperature, and carrying out heat preservation to obtain the high-temperature-resistant formaldehyde-free flame retardant. Depolymerizing the prepolymer to generate an alpha-cyanoacrylate crude product, and rectifying the crude product under reduced pressure to obtain the high-purity alpha-cyanoacrylate medical adhesive. Compared with the prior art, the preparation method has the advantages that the high-yield poly (alpha-cyanoacrylate) prepolymer can be prepared, and the prepared alpha-cyanoacrylate medical adhesive is high in yield and high in purity.

The invention discloses a preparation method of a medical intermediate 2-(4-nitrophenyl) butyric acid, and belongs to the technical field of medical fine chemical engineering. According to the method, p-nitrochlorobenzene and alkyl cyanoacetate are used as raw materials to react to prepare an intermediate 2-cyano-2-(4-nitrophenyl) acetoacetate, and then the intermediate 2-cyano-2-(4-nitrophenyl) acetoacetate reacts with diethyl sulfate under the alkaline condition to obtain the 2-cyano-2-(4-nitrophenyl) butyric acid alkyl ester. And finally, hydrolyzing through a concentrated sulfuric acid and acetic acid mixed system to obtain the 2-cyano-2-(4-nitrophenyl) butyric acid. The raw materials and reagents used in the method are cheap and easy to obtain, the process is simple and easy to implement, and the cost advantage is remarkable. Meanwhile, the adopted reaction route does not generate isomeride impurities such as 2-(2-nitrophenyl) butyric acid and the like, the yield is high, and the quality of the obtained product is good.

The preparation method comprises the following steps: reacting 7, 7 '-bis (methoxymethoxy)-1, 1'-spirobiindane with a configuration S or a configuration R with butyl lithium and ultra-dry DMF (Dimethyl Formamide), removing a protecting group from a crude product under the action of hydrochloric acid, and performing column chromatography to obtain the chiral self-assembled fluorescent probe with spirocoumarin characteristics. And carrying out condensation cyclization on the spirocoumarin with cyanoacetic acid, ammonium acetate and acetic acid to obtain the spirocoumarin chiral fluorescent probe with configuration S or configuration R. The chiral fluorescent probe with spirocoumarin characteristics is prepared for the first time, through the synergistic effect of spirochirality of 2, 2 ', 3, 3'-tetrahydro-1, 1 '-spirodi [1H-indene]-7, 7'-diol (SPINOL) and a coumarin fragment, not only is the selective recognition ability of the coumarin probe enhanced, but also the stability and sensitivity of the coumarin probe in a complex environment are improved, background noise is also reduced, and the fluorescent probe has good application prospects. Therefore, the detection sensitivity of the fluorescent probe is improved.

The invention discloses a modified lithium-rich manganese-based positive electrode material as well as a preparation method and application thereof, and belongs to the technical field of positive electrode materials. The preparation method comprises the following steps: (1) adding acid with high electronegativity into a solvent to obtain an acid solution; adding the MOF material into an acid solution, carrying out heating reaction for a set time, and carrying out solid-liquid separation to obtain an MOF material containing a high-electronegativity anion group; wherein the acid with high electronegativity is one or more of trifluoromethanesulfonic acid, trinitrobenzene sulfonic acid and cyanoacetic acid; and (2) mixing the MOF material containing the high electronegativity anion group with a lithium-rich manganese-based positive electrode material solid phase to obtain the modified lithium-rich manganese-based positive electrode material. The MOF material is treated by high-electronegativity acid and then is compounded with the lithium-rich manganese-based positive electrode material, so that the ion transmission rate of a positive electrode material interface can be effectively improved, the polarization phenomenon of the positive electrode material is reduced, and the rate capability of the material is improved.

The application discloses a preparation process of (1R, 5S)-6,6-dimethyl-3-azabicyclo[3.1.0]hexane, which comprises the following steps: taking 3-methyl-2-butenoic acid ethyl ester as a starting raw material, carrying out an electrophilic addition reaction with bromine in dichloromethane to obtain compound a; taking acetone as a solvent, and performing a removal reaction on the compound a in the presence of anhydrous potassium carbonate to obtain compound b; taking methanol as a solvent, adding sodium methoxide, adding 2-cyanoacetic acid ethyl ester into the system, and performing a nucleophilic addition reaction on the compound b to obtain compound c; taking dimethyl sulfoxide as a solvent, taking lithium chloride as a catalyst, and performing a deesterification reaction on the compound c in the presence of water to obtain compound d; taking methanol as a solvent, taking Raney nickel as a catalyst, adding 7M ammonia / methanol solution, and performing a cyclization reaction on the compound d to obtain compound e; and taking tetrahydrofuran as a solvent, taking lithium aluminum hydride as a catalyst, and reducing the compound e to obtain the product (1R, 5S)-6,6-dimethyl-3-azabicyclo[3.1.0]hexane.

The application belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of tetrahydrozoline. The tetrahydrozoline is synthesized from trifluoromethylaniline and 2-cyanoacetic acid ethyl ester under the action of an alkaline catalyst, the method has mild conditions, simple and easy-to-operate post-treatment and purification, low energy consumption, short working hours, and is suitable for large-scale production.

The application discloses a kind of overcharge-preventing lithium battery electrolyte and its preparation method in the technical field of lithium ion battery, the electrolyte uses the composite system of carbonate solvent and fluorine-containing solvent, cooperates mixed lithium salt and two new additives: difluorocyclohexyl benzothiazolium hexafluorophosphate and 2,4,6-tri (cyanoacetic acid methyl ester group) -1,3,5-triazine.The preparation process includes solvent mixing, lithium salt dissolving, additive adding and multi-step purification process.Two additives are prepared by oxidation cyclization, quaternary ammonium and esterification, condensation reaction.The electrolyte has high conductivity and lithium ion transference number, high oxidation potential, good thermal stability, can effectively inhibit electrolyte decomposition and metal ion dissolution under overcharge condition, significantly improves the high-voltage stability and safety of lithium battery, and is suitable for high-voltage lithium battery, electric vehicle power battery and large-scale energy storage system and other fields.

The invention relates to agomelatine as well as a crystal form and a preparation method thereof. The preparation method comprises the following steps: enabling 7-methoxy-1-tetralone and cyanoacetic acid to react in the presence of a catalytic amount of benzylammonium heptanoate under the condition of removing formed water, so as to obtain (7-methoxy-3, 4-dihydro-1-naphthyl) acetonitrile; in the presence of allyl methacrylate, enabling the previous product to react with a hydrogenation catalyst to obtain 7-methoxy-1-naphthyl acetonitrile; converting the nitrile compound into a primary amine; and treating the primary amine compound with acetic anhydride to obtain agomelatine separated in a solid form. The invention also provides a crystal form of agomelatine and application of agomelatine in preparation of a medicine for treating or preventing melatonin energy system diseases.