454 results about "Ethylamines" patented technology

The invention discloses an acetonitrile hydrogenation catalyst and a preparation method and application thereof. The acetonitrile hydrogenation catalyst is a transition metal modified Pt supported catalyst. A transition metal precursor adopted in the transition metal improvement is an oxide containing transition metal elements; the transition metal element is selected from at least one of titanium, vanadium, manganese, iron, cobalt, nickel and copper; the acetonitrile hydrogenation catalyst also comprises a carrier; the carrier is selected from at least one of gamma-Al2O3, SiO2, an MOR molecular sieve and a ZSM-5 molecular sieve. The catalyst can effectively catalyze acetonitrile hydrogenation to prepare ethylamine under mild reaction conditions. The supported catalyst provided by the invention has excellent reaction performance such as high acetonitrile conversion rate in acetonitrile hydrogenation reaction, the reaction condition is mild, the operation is simple, and the catalyst is easy to prepare and can be recycled.

The invention discloses a lithium battery negative electrode binder of modified carboxymethyl cellulose lithium, and belongs to the technical field of lithium ion batteries, and the modified carboxymethyl cellulose lithium is prepared by grafting carboxymethyl cellulose with an acrylic monomer and a sulfonic monomer, acidifying, lithiating, cross-linking with cystine, and carrying out surface modification with 2-(3, 4-dihydroxyphenyl) ethylamine. The preparation method comprises the following steps: grafting an acrylic monomer and a sulfonic monomer copolymerization long chain on a main chain of carboxymethyl cellulose, introducing additional carboxyl and sulfonic groups, and introducing cystine with a disulfide bond as a cross-linking agent and 2-(3, 4-dihydroxyphenyl) ethylamine with a catechol group as a tackifier to prepare modified carboxymethyl cellulose lithium; the lithium content of the obtained modified lithium carboxymethyl cellulose is higher than that of common lithium carboxymethyl cellulose, the adhesive property is enhanced, the toughness is improved, and the cycle performance is enhanced.

The invention discloses a method for preparing calcium hydroxide slurry with high specific surface area and high pore volume, which comprises the following steps: S1, adding an alcohol reagent into water to obtain a solution A; s2, adding an inorganic salt solution into the solution A, and uniformly mixing to obtain a solution B; s3, a reagent X is added into the solution B, ultrasonic mixing is performed to obtain a solution C, and the reagent X is a mixture of phenol or triethanolamine, ethidene diamine and ethylamine; and S4, adding calcium oxide powder into the solution C, continuously stirring, and reacting to obtain calcium hydroxide slurry. The invention provides a method for preparing calcium hydroxide slurry with high specific surface area and high pore volume, the calcium hydroxide slurry prepared by the method can form calcium hydroxide with high specific surface area and high pore volume when in use, and the method aims to solve the problems of low specific surface area and low pore volume of the existing calcium hydroxide. Therefore, the problem of desulfurization performance inactivation caused by blockage of calcium hydroxide (desulfurizer) pores by generated CaSO3 and CaSO4 in the desulfurization process is avoided.

The present invention discloses an imidazole derivative, a preparation method thereof, and an application, belonging to the field of organic chemistry. The preparation method of the imidazole derivative of the present invention includes: adding compound 2a and dimethyl sulfate into an organic solvent, heating and reacting to obtain compound 3a; wherein, compound 2a is prepared by adding compound 1a, TrtCl, and a base reagent into a solvent, controlling the temperature at 0-10 °C, mixing evenly and reacting. The present invention also further prepares 2-(1-methylimidazol-5-yl)ethylamine (4a) by using the imidazole derivative. The present invention selects dimethyl sulfate as a methylation reagent and cooperates with a specific protecting group design to achieve the efficient preparation of 2-(1-methylimidazol-5-yl)ethylamine, with a total yield of 82.4%.

The invention relates to a green preparation method of fluopyram intermediate 3-chloro-5-(trifluoromethyl)-2-ethylaminopyridine, which comprises the following steps: step 1, Ullmann reaction: coupling 3-chloro-2-methyl-5-trifluoromethylpyridine (C1) and N-bromomethyl phthalimide (C2) in the presence of a copper catalyst and potassium tert-butoxide to generate an intermediate (C3); and step 2, hydrolysis reaction: hydrolyzing the intermediate (C3) in the presence of hydrazine sulfate and an alkaline condition to generate the fluopyram intermediate 3-chloro-5-(trifluoromethyl)-2-ethylamino pyridine. The method has the advantages of short synthesis steps, easily available raw materials, no use of high-toxicity cyanogen compounds, low catalyst cost, difficult poisoning, recycling, simple post-treatment process, and less waste liquid generation, greatly reduces the production cost, improves the production safety, reduces the waste liquid discharge amount, and accords with the idea of green synthesis.

The invention relates to a nitrogen-containing heterocyclic compound as well as a preparation method and application thereof, belongs to the technical field of heterocyclic compound synthesis, and solves the problems of low reaction efficiency and high energy consumption caused by the fact that an existing method for synthesizing an indole maleimide derivative needs to be carried out step by step. The preparation method comprises the following steps: step 1, adding indoleacetamide and a nucleophilic reagent into a mixed solution, and reacting; 2, performing post-treatment to obtain a nitrogen-containing heterocyclic compound; the mixed solution comprises alkali, an additive and an organic solvent; the alkali comprises one of triethylamine (Et3N), N, N-diisopropylethylamine, pyridine and 1, 8-diazabicyclo [5.4. 0] undec-7-ene, and the alkali comprises one of 1, 8-diazabicyclo [5.4. 0] undec-7-ene.

The invention discloses a preparation method of a composite flocculant based on efficient water treatment, belongs to the technical field of flocculant processing, and aims to solve the technical problem that the flocculation performance and the settling performance of a flocculant need to be further improved in the prior art. The preparation method specifically comprises the following steps: putting acrylamide, diallyldimethylammonium chloride, 2-hydroxypropyl methacrylate and deionized water into a reaction kettle, and uniformly mixing to obtain a mixed monomer; according to the preparation method, citric acid monohydrate and iron nitrate nonahydrate react under a mild acidic condition to form a Fe < 3 + >-citric acid complex, and then 2-hydroxyethylamine is introduced to further participate in complexing to obtain a citric acid complexing solution, so that not only is the flocculation performance of the composite flocculant improved, but also the settling performance of the composite flocculant is improved.

The invention provides application of a CsZAT6 gene or protein in regulation and control of theanine synthesis, and belongs to the technical field of molecular breeding. According to the application of the CsZAT6 gene or the encoding protein of the CsZAT6 gene in regulation and control of theanine synthesis, specifically, the synthesis of theanine is reduced by negatively regulating and controlling the expression level of the CsZAT6 gene, or the synthesis of theanine is promoted by positively regulating and controlling the expression level of the CsZAT6 gene. The CsZAT6 gene is a potential target gene for synthesizing the theanine. Experimental results show that the CsZAT6 gene can respond to IAA treatment, and the content of ethylamine and theanine is regulated and controlled in a tea tree body by regulating and controlling a CsAlaDC promoter.

The invention provides a cross-linking and curing environment-friendly polyurethane waterproof coating and a preparation method thereof, and the cross-linking and curing environment-friendly polyurethane waterproof coating comprises the following raw materials by weight: 15-30 parts of a polyhydroxy compound; 6 to 15 parts of pentaerythritol polyether; 1-5 parts of an anionic surfactant; 1 to 5 parts of nano silicon dioxide aerogel; 1-8 parts of wollastonite powder; 25 to 45 parts of fly ash floating beads; 10 to 25 parts of diisocyanate; 0.5 to 3 parts of chlorinated paraffin; and 0.5 to 3 parts of N, N-dimethyl-2-hydroxyethylamine. The cross-linking curing environment-friendly polyurethane waterproof coating provided by the invention solves the environment-friendly problem of the traditional polyurethane waterproof coating, realizes solvent-free curing, meets the environment-friendly requirement, improves the comprehensive properties such as elasticity and durability of a coating film, and provides a safer and more effective solution for waterproof construction.

The invention discloses a method for enriching a sulfydryl-containing peptide fragment based on covalent binding, in the method, a chemical reagent, namely 2-(2-pyridyl disulfide) ethylamine, capable of reacting with sulfydryl is used, the reagent comprises two functional reactive groups, specifically, amino and pyridyl disulfide, the amino can react with carboxyl magnetic beads, and the sulfydryl-containing peptide fragment can react with carboxyl magnetic beads. A novel pyridine disulfide-based magnetic bead material, namely the pyridine disulfide-based agar magnetic bead, is formed. According to the method, pyridine disulfide can directly react with the sulfydryl peptide fragment to form a covalent bond, so that the enrichment of the sulfydryl peptide fragment is realized, the sulfydryl peptide fragment can be eluted by adding a reducing agent such as DTT, and the method has the characteristics of low cost, good selectivity and the like.

The invention provides a method for preparing a nitrogen, phosphorus and sulfur tri-doped hollow carbon nanocage material derived from a covalent triazine polymer. The method comprises the following steps: by taking zinc nitrate hexahydrate and 2-methylimidazole as reactants and methanol as a solvent, stirring at room temperature to synthesize ZIF-8; the preparation method comprises the following steps: by taking phosphonitrilic chloride trimer and bisphenol S as monomers and ZIF-8 as a template agent, carrying out polymerization under the induction of an N, N-diisopropylethylamine initiator so as to generate ZIF-8 (at) PZS; and performing high-temperature pyrolysis to synthesize the nitrogen, phosphorus and sulfur triple-doped hollow carbon nanocage material. The invention also discusses the application of the nitrogen, phosphorus and sulfur tri-doped hollow carbon nanocage material in an air electrode material of a zinc-air battery. Meanwhile, the conductivity and the oxygen reduction reaction electro-catalytic performance of the obtained carbon material are remarkably improved through the nitrogen, phosphorus and sulfur doped synergistic effect, the half-wave potential of the carbon material reaches up to 0.85 V vs. RHE, and the limiting current density can reach 5.19 mA cm. A zinc-air battery assembled by using the material as an air electrode shows high peak power density of 194 mW cm.

The invention provides a fluorine-containing polymer wetting reversal agent suitable for shale reservoir protection as well as a preparation method and application of the fluorine-containing polymer wetting reversal agent. The preparation method of the reverse wetting agent comprises the following steps: adding ethylamine, triethylamine and deionized water into a reaction flask, and adding perfluorooctanoyl chloride into the system for reaction; after the reaction is completed, potassium hydroxide and 2-chloroethanol are continuously added for reaction; and after the reaction is completed, obtaining the N-ethyl-N-hydroxyethyl perfluorooctanamide. Adding nanoparticles, a silane coupling agent and ammonia water into the dispersant solution, and carrying out a modification reaction to obtain a modified nanoparticle solution; and adjusting the pH value of the obtained modified nanoparticle solution to 5-9, adding N-ethyl-N-hydroxyethyl perfluorooctanamide, introducing nitrogen to remove oxygen, adding an initiator, and carrying out thermal initiation polymerization reaction to obtain the composite material. The wetting reversal agent disclosed by the invention has excellent wetting reversal performance and a certain filtration reduction effect, and provides innovative thinking for development of a high-performance water-based drilling fluid technology.

The invention discloses a triazine desulfurizer and a preparation method thereof, and belongs to the technical field of gas purification. The triazine desulfurizer is mainly prepared from the following raw materials in percentage by weight: 20 to 50 weight percent of triazine derivative, 10 to 15 weight percent of sterically hindered amine, 3 to 7 weight percent of stabilizer, 1 to 3 weight percent of synergist, 0.5 to 1.5 weight percent of penetrant, 0.5 to 1.5 weight percent of inhibitor, 1 to 2 weight percent of additive and the balance of water, the preparation method of the triazine derivative comprises the following steps: adding 2-(diphenylphosphino) ethylamine into a toluene solvent, adding a paraformaldehyde aqueous solution in batches under a stirring condition, and reacting for 2-8 hours to obtain the triazine derivative. According to the triazine desulfurizer and the preparation method thereof provided by the invention, the triazine derivative and the sterically hindered amine are taken as a host, and the stabilizer, the synergist, the penetrant, the inhibitor and the assistant are compounded, so that the scaling trend of the triazine desulfurizer in an oil and gas well can be slowed down, the dissolution rate of hydrogen sulfide and the mass transfer rate in a solution are increased, and the desulfurization reaction is promoted; the desulfurization effect and the desulfurization rate are improved, and meanwhile, a very good scale inhibition effect is also achieved.

The invention discloses a preparation process of berberine hydrochloride, and belongs to the technical field of berberine production. The invention relates to a berberine hydrochloride preparation process, which comprises: S1, mixing a ferric sulfate-aluminum sulfate composite salt, sodium chloride, zinc chloride and anhydrous formic acid, pre-activating, adding N-2, 3-dimethoxybenzyl homopiperony lamine hydrochloride, dropwise adding a glyoxal mixed solution, and carrying out a reflux reaction. And S2, cooling the reaction liquid until a solid is separated out, filtering, adding a filter cake and diatomite into purified water, stirring, adjusting alkali, heating, and continuously stirring for 0.5-1 hour. Cooling and filtering, and reserving filtrate; s3, adjusting the acidity of the filtrate, cooling and growing crystals; and filtering, rinsing a filter cake, and carrying out vacuum drying on the filter cake to obtain berberine hydrochloride. The berberine hydrochloride prepared by the method is high in yield and purity, and the preparation process is safe, short in flow and friendly to human bodies and environment.

The invention relates to a preparation and synthesis method of an amino-substituted nitrogen-containing heterocyclic ring, which is carried out by using an ice bath auxiliary device, and is characterized by comprising the following steps: adding p-aminobenzaldehyde into a toluene solution of aminoacetaldehyde dimethyl acetal, heating to reflux to obtain (Z)-N-(4-acetamido-benzylidene)-2, 2-dimethoxyethylamine, and reacting for 2-4 hours to obtain the N-(4-acetamido-benzylidene)-2, 2-dimethoxyethylamine. And carrying out three steps to obtain the 6-aminoisoquinoline. Wherein the reaction liquid is poured into the crushed ice, an ice bath auxiliary device is used for implementing, and the ice bath auxiliary device comprises an ice crusher (1), a carrying table (2), a heating plate array (3) and a tray (4).

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a preparation method and application of an impurity of a beta2 adrenal receptor stimulant and M receptor antagonist bifunctional active compound. According to the impurity preparation method of the beta2 adrenal receptor stimulant and M receptor antagonist bifunctional active compound, acetylation of amino is successfully realized by using acetylation reagents such as acetyl chloride and alkali accelerators such as N, N-diisopropylethylamine, then debenzylation is performed through hydrogenation reaction, and the compound shown in the formula I is successfully prepared. Then, through liquid chromatography purification, a high-purity compound as shown in the formula I is obtained, and the raw material medicine as shown in JKN2304 can meet the requirements of reference substances in the research and development process; the technical problem that in the prior art, an impurity synthesis process of a beta 2 adrenal gland receptor agonist and M receptor antagonist bifunctional active compound is lacked is solved.

The invention discloses a high-strength energetic compound based on a polydopamine and thiourea polymer and a preparation method of the high-strength energetic compound, and the energetic compound is composed of energetic crystal 1, 3, 5-triamino-2, 4, 6-trinitrobenzene, the polydopamine and the thiourea polymer. The preparation method comprises the following steps: modifying an energetic crystal 1, 3, 5-triamino-2, 4, 6-trinitrobenzene through polydopamine in advance; the polythiourea is obtained through reaction of 2, 2 '-(ethylene dioxygen) diethylamine, carbon disulfide and trimethylolpropane tripolypropylene glycol ether, and the addition amount is 2.5 wt.%-10 wt.%; and mixing the two components by a kneading method, and drying to obtain the energetic compound. The obtained compound has the characteristics of strengthening and toughening, the Brazil mechanical strength reaches 14.76 MPa, and the fracture strain reaches 0.474%. By introducing polyphenol polydopamine and polythiourea to achieve a synergistic effect, the mechanical property of the explosive is greatly improved, and a technical support can be provided for the application of the explosive; meanwhile, the preparation method is simple, mild in reaction condition and easy for large-scale production.

The invention relates to a solid electrolyte of organic-inorganic hybrid halogen compound molecules, preparation thereof and an all-solid-state battery, and belongs to the technical field of energy storage batteries. The chemical general formula of the solid electrolyte is MaNb + eQcXdYa + bn + cq + dxZen or MaN2b + eQcXdYa + cq + dxZenObn, wherein M is selected from one of methylamine, ethylamine, propylamine, butylamine, aniline, benzylamine and phenylethylamine; n, Q and X are different metal elements; y is selected from halogen; z is a pseudohalide ion; the value range of a, b, c, d and e is 0 lt; a < = 3, 0lt; b < = 3, 0lt; c < = 1, 0lt; d < = 1, 0lt; e < = 6; and n, q and x are values of valences of the N element, the Q element and the X element respectively. The electrolyte material disclosed by the invention has high ionic conductivity, good flexibility and machinability and excellent air stability, and a battery formed by the solid electrolyte material has excellent electrochemical performance.

The invention discloses a preparation method of a near-infrared two-region fluorescently-labeled phospholipid molecule and a preparation method of a lipid nano-carrier of the phospholipid molecule, and relates to the field of preparation methods of cyanine dyes. The invention aims to solve the technical problems that the application of the organic cyanine dye in a living body is limited by the hydrophobicity of the organic cyanine dye and the fluorescence intensity is low due to the aggregation quenching effect of the organic cyanine dye. The method comprises the following steps: preparing a compound 2 from 1, 8-naphthalimide and iodohexane, and then preparing C6 from the compound 2, 2-chloro-3-(hydroxymethylene)-1-cyclohexene-1-formaldehyde and sodium acetate; then C6 and mercaptobenzoic acid are used for preparing C6-COOH; the preparation method comprises the following steps: preparing C6-Lipid from N, N-diisopropylethylamine, HBTU, C6-COOH and 4-(1, 2, 2-triphenylvinyl) aniline by virtue of a hydrothermal method; the preparation method comprises the following steps: preparing a lipid nano-carrier from C6-Lipid, DMPC (Dimethyl Pyrrolidone), DOPE (Dioctyl Olefin Polyethylene) and According to the phospholipid molecule and the lipid nano-carrier thereof prepared by the invention, effective imaging of fluorophores is realized, and aggregates such as J aggregation and the like are possibly generated, so that the fluorescence quantum yield is improved, and an efficient fluorescence imaging effect is achieved. The cyanine dye prepared by the invention is used for fluorescence imaging.

The invention discloses a modified polypeptide as well as a preparation method and application thereof, the preparation method comprises the following steps: on the basis of solid-phase synthesis of RADA16, 1-hydroxybenzotriazole and benzotriazole-N, N, N ', N'-tetramethylurea hexafluorophosphate are adopted as condensing agents, N, N-diisopropylethylamine-containing N, N-diisopropylethylamine is added into the condensing agents, and a reaction is carried out for 2-4 hours to obtain the modified polypeptide. And adding amino-terminated or carboxyl-terminated polyethylene glycol or amino-containing chitosan oligosaccharide into N, N-dimethylformamide for condensation, cutting polypeptide from the resin after the reaction is completed, precipitating, washing, re-dissolving and freeze-drying to obtain the polypeptide. The polypeptide provided by the invention has the characteristic of forming hydrogel through self-assembly in a specific medium, and the gel forming time of the polypeptide is within 21-60 seconds and is obviously faster than that of RADA peptide (gel forming in 150 seconds) under the same condition; the polypeptide modified by the polyethylene glycol or the chitosan oligosaccharide can spontaneously form gel after being injected into the blood vessel so as to embolize the blood vessel, and the embolism is long in stabilization time and stable, and meets the actual clinical requirements.

The invention discloses a flue gas desulfurization composite synergist and a preparation method thereof, and relates to the technical field of flue gas desulfurization. The desulfurization composite synergist is prepared from the following raw materials in parts by weight: 5 to 10 parts of citric acid, 20 to 30 parts of binary acid, 15 to 20 parts of sodium formate, 15 to 20 parts of sodium salt, 12 to 18 parts of magnesium salt, 2 to 4 parts of surfactant, 2 to 4 parts of pH buffering agent and 5 to 10 parts of calcium oxide. The preparation method comprises the following steps: carrying out a ring-opening reaction on 3-(2-aminoethylamine) propyl methyl dimethoxy silane and glucolactone to obtain an intermediate 1, and then carrying out a two-step quaternization reaction to synthesize the novel surfactant. The prepared desulfurization composite synergist has a good desulfurization effect and is suitable for limestone-gypsum wet flue gas desulfurization.

The invention relates to an organic crystalline piezoelectric material based on chiral 4-bromophenylethylamine hydrochloride, which is synthesized by using hydrochloric acid as an anion and protonated (R / S)-4-bromophenylethylamine as a cation according to the stoichiometric ratio of (R / S)-4-bromophenylethylamine to hydrochloric acid of 1: 1. The invention provides an organic crystalline piezoelectric material based on chiral 4-bromophenylethylamine hydrochloride and a preparation method, and provides a two-dimensional hydrogen bond network construction strategy based on protonated chiral amine: protonated (R / S)-4-bromophenylethylamine cations are used as structural elements, chloride ions are used as charge balance bodies, and the chiral 4-bromophenylethylamine hydrochloride is prepared by precisely regulating the interaction of intermolecular hydrogen bonds. Constructing a two-dimensional hydrogen bond network with high orientation; by enhancing ordered arrangement of molecular dipoles and optimizing a lattice strain-polarization response collaborative mode, breakthrough improvement of piezoelectric performance is successfully realized, and a new normal form is provided for developing high-performance organic piezoelectric materials.

The invention relates to the field of cosmetics, in particular to a blue copper peptide composition with instantaneous cool feeling and infiltration promotion effects and a preparation method and application of the blue copper peptide composition. The composition comprises an active component copper-blue peptide and a cooling and permeation enhancing system formed by compounding at least two of menthane formylethylamine, menthone glyceryl ketal and methyl diisopropyl propionamide, and the active component can further comprise hexapeptide-11, a blue algae extract and a yeast fermentation product. The preparation method of the composition comprises three core steps of providing a water phase, adding the active ingredients and adding the cool and refreshing infiltration promoting system and other components. Through synergistic compounding of specific fresheners, on the premise that the use amount of each single component is remarkably reduced, efficient permeation promotion of the copper-blue peptide is achieved, the layered cool feeling experience which takes effect quickly and is lasting and mild is provided, the common skin irritation problem of a traditional permeation promoter or a high-concentration single freshener is avoided, and the effect is remarkable. And the transdermal patch has excellent transdermal efficiency, active matter stability and use comfort.

The invention relates to the technical field of preparation of cupanicilib, and discloses a novel preparation method of cupanicilib, which comprises the following steps: by taking vanillic acid as an initial raw material, carrying out methyl esterification, nitration, alkylation reaction with N-3-chloropropylmorpholine hydrochloride, ester group hydrolysis, condensation with urea, nitro reduction, intramolecular condensation and condensation with chloroethylamine hydrochloride to obtain cupanicilib. According to the synthetic scheme, the synthetic route is short, the raw materials are easy to obtain, the yield is high, no dangerous reaction process exists in the reaction process, a highly toxic reagent is not used, and the synthetic scheme is green and efficient.

The invention belongs to the field of pesticide preparation, and particularly relates to an improved preparation method of 2-(2 '-bromomethyl phenyl)-2-carbonyl methyl acetate. 2-oxo-2-(o-tolyl) ethyl acetate is used as a raw material and is sequentially subjected to oximation reaction, structure transposition treatment, bromination reaction and polybrominated substance to monobromination reaction, and finally 2-(2 '-bromomethyl phenyl)-2-carbonyl methyl acetate is obtained. Wherein the structure transposition treatment comprises the following steps: by taking an oximation product as a substrate, introducing a catalyst under a system anhydrous condition to realize conversion from a Z configuration to an E configuration; the polybrominated substance to monobrominated product conversion reaction comprises the following steps: dissolving a brominated product in THF, then adding dimethyl phosphite and diisopropylethylamine, and carrying out a reaction to realize conversion of the polybrominated substance into a monobrominated product. According to the method, the conversion of polybrominated substance impurities into monobrominated products is optimized through process improvement, so that the yield of the target product is improved, and the method is simple to operate, few in by-products and suitable for industrial production.

The invention relates to a method for simply and conveniently preparing high-purity lotinia, which comprises the following steps of: reacting 5-acetyl-3-methyl-2-thiophenecarboxylic acid with 2, 2, 2-trifluoro-1-trichlorophenyl ethyl-1-ketone to obtain 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-formic acid, and reacting the 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-formic acid with 2, 2, 2-trifluoro-1-trichlorophenyl ethyl-1-ketone to obtain 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-carboxylic acid. Reacting the isoxazole thiophene formic acid compound with hydroxylamine hydrochloride to obtain an isoxazole thiophene formic acid compound; the preparation method comprises the following steps: reacting 5-[(5S)-5-trichlorophenyl-5-trifluoromethyl-4, 5-dihydro-isoxazole-3-yl]-3-methyl-thiophene-2-formic acid with (R)-1-(p-tolyl) ethyl-1-amine to obtain 5-[(5S)-5-trichlorophenyl-5-trifluoromethyl-4, 5-dihydro-isoxazole-3-yl]-3-methyl-thiophene-2-formic acid; and finally, carrying out condensation on the product and 2-amino-N-trifluoroethyl acetamide hydrochloride, so as to obtain the (5S)-configuration final product lotinib. The method has the advantages of short synthetic route, simple process, mild reaction and high chiral purity and HPLC purity, and is especially suitable for large-scale production.

To provide a fine granulated agent replenishing liquid for a plating liquid, with the replenishing liquid being excellent in the initial stability and safety, and the replenished plating liquid being excellent in the aging stability, without damaging the appearance of a plating film when replenished for a long period of time nor dissolving an organic resist film present on a material to be plated.SOLUTION: A fine granulated agent replenishing liquid for a plating liquid, replenishing a fine granulated agent to a tin-based plating solution including one or two or more kinds of compounds selected from the group consisting of benzaldehyde, 1-naphthaldehyde, 1-naphthoic acid, 1-acetonaphthone, DL-1-(1-naphthyl)ethylamine, and benzylidene acetone, includes a phenyl glycol-based surfactant, the fine granulated agent and water, with a content of the fine granulated agent therein being in a range of 0.1 g / L or more and 10.0 g / L or less, a content of the phenyl glycol-based surfactant therein being in a range of 5 g / L more and 50 g / L or less, and a content of alcohol being less than 1 mass%.SELECTED DRAWING: None

The application discloses a preparation method of enciferstat bulk drug and belongs to the field of drug synthesis. 9,10-dimethoxy-2-(2,4,6-trimethylphenylimino)-3,4,6,7-tetrahydro-2H-pyrimido[6,1-a]isoquinolin-4-one (SM) is used as a raw material, and the raw material is reacted with cyclohexylamine under alkaline conditions, and the reaction is washed with water, dried, and concentrated to obtain an intermediate I; the intermediate I is reacted with urea under pressurized heating conditions to prepare an enciferstat drug molecule, the two-step yield is more than 67%, and the purity is more than 99%, the method has a simple operation process, the product is easy to purify, the yield is high, the product purity is high, and a new method for preparing enciferstat bulk drug is provided.

This invention belongs to the field of two-dimensional material preparation technology, and provides an MXene material and its preparation method. The preparation method of the MXene material includes: mixing a MAX phase precursor to be etched with an organic halide reagent and a morphology modifier, performing a solvothermal etching reaction, and after the reaction, washing and drying the resulting product to obtain the MXene material; wherein the organic halide reagent is triethylamine trihydrofluoride, triethylamine hydrochloride, or dichloroethylamine hydrochloride, and the morphology modifier is ethylene glycol, dimethyl sulfoxide, or cyclohexane. The method of this invention can effectively control the microstructure and pore structure of the MXene material.

The present invention discloses an electrochemiluminescent compound, a preparation method thereof and an application thereof, wherein the structural formula of the electrochemiluminescent compound is: wherein n is 100-200, R1, R2, R3 and R4 are all selected from one of a Y group and a hydrogen group, and at least one of R1, R2, R3 and R4 is a Y group. The preparation method of the electrochemiluminescent compound comprises the following steps: dissolving an iridium-containing complex, N, N-diisopropylethylamine, N, N, N', N'-tetramethyl-O-(N-succinimide) urea tetrafluoroborate in N, N-dimethylformamide and mixing; adding a polyethyleneimine solution, performing an amide reaction, separating, and obtaining the electrochemiluminescent compound. The electrochemiluminescent compound (Ir-PEI) of the present invention can improve the water solubility of the iridium-containing complex, can also be used as a coreactant unit in the molecule to promote the generation of ECL signals, and can be used as an ECL active material to construct and prepare an iridium ECL reagent.