2905 results about "Organic synthesis" patented technology

The application provides a process method for preparing (2-(3,6-dimethoxy-9H-carbazol-9-yl)ethyl) phosphonic acid, and particularly relates to the technical field of organic synthesis. The process method is that, under alkaline conditions, a halogenated phosphonate compound is added into a 3,6-dimethoxy-9H-carbazole solution to perform a reaction, hydrochloric acid aqueous solution is added after the reaction to perform acidolysis degreasing, and finally (2-(3,6-dimethoxy-9H-carbazol-9-yl)ethyl) phosphonic acid is obtained through extraction, reflux adsorption and beating purification. The process method uses 3,6-dimethoxy-9H-carbazole as a starting material, realizes the synthesis of the target product through one-pot reaction, has mild reaction conditions, uses non-toxic raw materials which are easy to obtain, has simple synthesis process, is convenient to operate, and has high separation yield.

The invention belongs to the technical field of organic synthesis, and particularly discloses an ammonia aromatic alkene modified near-infrared BODIPY fluorescent probe as well as a preparation method and application thereof.The near-infrared BODIPY fluorescent probe is obtained by adopting 6-(dimethylamino) nicotinic aldehyde to directionally modify the alpha position of BODIPY and constructing an expanded conjugated system through Knoevenagel condensation. Wherein dimethylamino provides a strong electron donating effect, a molecular structure is twisted into a non-planar configuration due to steric hindrance of a pyridine ring, pi-pi accumulation is reduced, and an ACQ effect is inhibited. According to the structural modification strategy, significant red shift of absorption / emission wavelength is realized by expanding a molecular pi-conjugated skeleton, and meanwhile, the stability of the BODIPY core and the quantum yield are effectively enhanced. The probe molecule can specifically recognize the diphenylalanine dipeptide structural unit by utilizing the synergistic coordination effect of the 2-aminopyridine derivative and the BODIPY mother nucleus, so that the selective detection of the Alzheimer's disease biomarker Abeta42 is realized, and a novel optical detection tool is provided for the early molecular diagnosis and targeted therapy of AD (Alzheimer's disease).

The invention discloses a synthesis method of bromo-triazine, which belongs to the technical field of organic synthesis, and comprises the following steps: preparing an alumina-loaded N, N-dimethylaminopyridine catalyst, filling the alumina-loaded N, N-dimethylaminopyridine catalyst in a fixed bed reactor, introducing tribromophenol and metal oxide mixed slurry and cyanuric chloride slurry, carrying out a reaction for 2-4 hours, and carrying out a reaction for 2-4 hours to obtain the bromo-triazine. Raising the temperature for reaction to obtain a crude product solution; and performing post-treatment to obtain a bromo-triazine product. According to the invention, the aluminum oxide loaded N, N-dimethylaminopyridine catalyst is synthesized, and the N, N-dimethylaminopyridine enables the reaction speed to be higher and the yield to be higher; nano aluminum oxide is adopted for loading, so that on one hand, dealkalization synthesis of bromotriazine is realized, and on the other hand, the reaction efficiency is accelerated; the continuous process realizes non-aqueous medium and low-temperature short-time reaction, so that hydrolysis is further avoided; the aluminum oxide loaded N, N-dimethylaminopyridine catalyst is high in activity and stability, the synthesis method is simplified, and the aluminum oxide loaded N, N-dimethylaminopyridine catalyst is suitable for industrial large-scale production.

A method for continuously producing m-xylylenediamine belongs to the technical field of organic synthesis and comprises the following steps: (1) mixing isophthalonitrile, toluene and liquid ammonia according to a mass ratio of 1: (3-5): (13-17) in a nitrogen atmosphere to form a reaction mixture; (2) heating the interior of a reaction bed containing a catalyst to 90-95 DEG C, continuously introducing hydrogen into the reaction bed, introducing the reaction mixture after the pressure intensity of the reaction bed is stable, and carrying out a catalytic hydrogenation reaction to generate a reaction product; and (3) carrying out gas-liquid separation on the reaction product, removing liquid ammonia from the liquid-phase product through an ammonia distillation process, and separating toluene and m-xylylenediamine through a rectification process to obtain m-xylylenediamine. According to the method, isophthalonitrile and hydrogen are used as raw materials, liquid ammonia and methylbenzene are used as reaction solvents, the raw materials and the reaction solvents are heated to 90-95 DEG C under the catalytic action of a catalyst for an exothermic reaction, m-xylylenediamine is generated through the reaction, and the reaction yield is larger than 99%.

The invention relates to the technical field of organic synthesis, and discloses a preparation process of (S)-3-aminobutyronitrile hydrochloride, which comprises the following steps: by taking a compound S1 as an initial raw material, sequentially implementing chlorination, amino protection, cyano substitution and deprotection reaction through four-step continuous reaction (M01 preparation, M02 preparation, M03 preparation and M04 preparation), and finally obtaining the high-purity (S)-3-aminobutyronitrile hydrochloride. The preparation process disclosed by the invention is simple and convenient to operate, mild in reaction condition, stable in yield of each step, high in safety and suitable for industrial large-scale production, and can be used for carrying out standard treatment on the cyanide-containing wastewater, and has a relatively good application prospect.

The invention relates to the field of organic synthesis, in particular to a synthetic method of 1-(2, 6, 6-trimethyl-1, 3-cyclohexadiene-1-yl) ethanone, and particularly relates to a synthetic method of 1-(2, 6, 6-trimethyl-1, 3-cyclohexadiene-1-yl) ethanone by taking 4-acetyl-3, 5, 5-trimethylcyclohexene as a raw material and carrying out bromination and elimination steps to synthesize the 1-(2, 6, 6-trimethyl-1, 3-cyclohexadiene-1-yl) ethanone. The method has the advantages of easily available raw materials and high reaction yield, and can be industrially implemented on a large scale.

The invention discloses a phenanthridine-6-formaldehyde derivative and a preparation method and application thereof.The preparation method comprises the steps that 2, 4, 5, 6-tetra (9-carbazolyl)-isophthalonitrile serves as a photocatalyst, 1-azabicyclo [2.2. 2] octane serves as a hydrogen atom transfer catalyst, a biphenyl isocyanide compound, the photocatalyst, the hydrogen atom transfer catalyst and an alkali additive are jointly dissolved in 1, 3-dioxolane, the mixture is stirred to be uniform, and the phenanthridine-6-formaldehyde derivative is obtained. And carrying out free radical tandem cyclization and acid-catalyzed hydrolysis reaction to obtain the phenanthridine-6-formaldehyde derivative. The invention also provides a specific reaction equation. According to the developed synthesis method of the phenanthridine-6-formaldehyde derivative, the compound can be efficiently and conveniently prepared, the technical bottlenecks of harsh reaction conditions and tedious steps in a traditional process are successfully overcome, raw materials which are low in price and easy to obtain are adopted, operation is carried out under mild conditions, the synthesis method has the outstanding advantages of being high in yield, safe and simple to operate, environmentally friendly and the like, and the method is suitable for industrial production. Good industrial application potential is shown.

The invention provides a preparation method of a bexagliflozin intermediate, and relates to the technical field of organic synthesis. The preparation method provided by the invention comprises the following steps: S1, substitution reaction: under the action of alkali, carrying out substitution reaction on 2-(cyclopropoxy) ethanol and a compound III ((5-halogen-2-chlorphenyl) (4-halophenyl) ketone) to generate a compound II; s2, reduction reaction: under the action of lewis acid, carrying out reduction reaction on a reducing agent and a compound II ((5-halogen-2-chlorphenyl) (4-(2-(cyclopropoxy) ethyoxyl) phenyl) ketone) to generate a compound I; the method has the advantages of mild reaction conditions, high atom utilization rate, high yield, high product quality and the like.

The invention relates to the field of organic synthesis, in particular to a method for preparing amorphous tigorazan through an anti-solvent recrystallization method, which comprises the following steps: dissolving tigorazan in 1, 4-dioxane to obtain a mixed solution, dropwise adding n-heptane into the mixed solution, stirring, crystallizing, filtering and drying to obtain the amorphous tigorazan. The method disclosed by the invention has the advantages of short preparation period, relatively low temperature requirement, high yield, strong impurity removal capability, low solvent residue and good product stability, and is high in industrial production value.

The invention relates to a molecular tag DMDPM compound, a preparation method thereof and application of the molecular tag DMDPM compound in assisting homogeneous synthesis of heptapeptide H6K, and belongs to the technical field of organic synthesis. The molecular tag DMDPM compound is 2, 4-dimethoxy-4 '-diphenylphosphinyl oxydiphenyl alcohol, and the molecular tag DMDPM compound is 2, 4-dimethoxy-4'-diphenylphosphinyl The method has the advantages of a liquid-phase synthesis method and a solid-phase synthesis method, H6K can be simply, quickly, economically and efficiently synthesized and prepared, and a 2, 4-dimethoxy-4 '-diphenylphosphinyloxy diphenyl alcohol small-molecule auxiliary group (also called as a carrier) can be recycled and directly reused, so that raw material waste is reduced, waste pollution is reduced, the cost is saved, and environmental protection is facilitated.

The invention belongs to the technical field of organic synthesis, and particularly relates to an asymmetric phenanthroline compound as well as a preparation method and application thereof. Compared with the original symmetric ligand compound, the asymmetric phenanthroline compound provided by the invention has the advantage that the extraction performance and selectivity of americium are improved. In addition, the asymmetric phenanthroline compound provided by the invention is stable in structure, has good acid resistance and radiation resistance, can be suitable for high-acidity post-treatment waste liquid, improves the fat solubility of the phenanthroline ligand, is easy to split phases, does not need to use 2-bromohexanoic acid and other synergistic extractants, and reduces the introduction of secondary wastes in the post-treatment process.

A technology for preparing glutaraldehyde through cyclopentene oxidation belongs to the technical field of organic synthesis, glutaraldehyde is prepared through cyclopentene oxidation by adopting a photocatalysis-electrocatalysis synergistic catalyst g-C3N4 / TiO2 (at) Au-Co / N-G. The catalyst is of a unique core-shell structure, is stable in property, promotes an oxygen reduction reaction in a catalysis technology, and has good catalytic activity. The conversion rate of cyclopentene and the selectivity of glutaraldehyde are remarkably improved, and the effect is remarkable.

The invention relates to the technical field of organic synthesis, in particular to 1-chloro-8-fluorine-7-isopropyl benzofuro [2, 3-c] pyridine as well as a synthesis method and an application of the 1-chloro-8-fluorine-7-isopropyl benzofuro [2, 3-c] pyridine. According to the invention, 1-chloro-8-fluoro-7-isopropyl benzofuro [2, 3-c] pyridine and nanogold are cooperated to cover the surface of a glassy carbon electrode (GCE), and a novel electrochemical modified electrode AuNPs / 1 / GCE is developed. The modified glassy carbon electrode shows good selectivity, high stability and sensitivity and wide detection range on the detection of the antibiotic furacilin.

The invention belongs to the field of organic synthetic chemistry, and relates to a preparation method of melatonin and meerythrine indole derivatives and compounds. Specifically, the indole derivative is efficiently synthesized by taking arylamine and carboxylic acid as raw materials through a one-pot two-step reaction in the presence of catalysis of ferric chloride hexahydrate (FeCl3. 6H2O), a ligand, a diazotization reagent, an additive and a solvent under the conditions of visible light irradiation, inert atmosphere and room temperature. According to the method, visible light induced iron-based LMCT catalysis and iron lewis acid catalysis functions are integrated, and efficient integration of diazotization, decarboxylation, free radical coupling and cyclization reaction is achieved. The method has the advantages that raw materials are cheap and easy to obtain, reaction conditions are mild, substrate applicability is wide, functional group compatibility is good, operation is easy, convenient and safe, and environment friendliness is achieved, gram-level scale preparation can be achieved, and a green and efficient synthesis path is provided for indole compounds with biological activity such as melatonin and meerythrine.

The invention relates to a high-water-solubility denitroflavin covalent complex as well as a preparation method and application thereof, and belongs to the technical field of organic synthesis and medicinal chemistry. Comprising the following steps: (1) firstly, carrying out bromination reaction on 3-methyl-10-ethyl denitroflavin, so as to obtain 3-methyl-10-(1-bromoethyl) denitroflavin; and (2) coupling the 3-methyl-10-(1-bromoethyl) denitroflavin with vitamin C, so as to obtain the high-water-solubility denitroflavin covalent complex. According to the present invention, the prepared highly water-soluble denitrificin covalent complex has the two-phase solubility of the organic solvent and the water, such that the water solubility of the 3-methyl-10-ethyl-denitrificin is substantially enhanced, and the application range of the denitrificin is expanded. And meanwhile, the denitrified flavin covalent compound also has good antioxidant activity, and the antioxidant duration can be prolonged.

The invention relates to the technical field of organic synthesis, and particularly discloses a synthesis process of 2-chloronicotinic acid. The synthesis process of the 2-chloronicotinic acid comprises the following steps: S1, mixing water, concentrated sulfuric acid, 3-cyanopyridine and a composite catalyst, performing pre-reaction, adding hydrogen peroxide, performing oxidation reaction, adjusting pH, performing solid-liquid separation, and washing to obtain an oxide intermediate; s2, in an inert atmosphere, adding phosphorus oxychloride into a reactor, adding the oxide intermediate and triethylamine for a chlorination reaction, recovering phosphorus oxychloride after the reaction is finished, hydrolyzing remaining materials, and performing solid-liquid separation and washing to obtain chloride; and S3, carrying out alkali dissolution, neutralization, decoloration and acidification on the chloride, carrying out solid-liquid separation, washing, carrying out secondary alkali dissolution, neutralization and secondary decoloration, adding a complexing agent, carrying out secondary acidification, carrying out solid-liquid separation, washing, drying and crushing to obtain the 2-chloronicotinic acid. The 2-chloronicotinic acid prepared by the method disclosed by the invention has relatively high purity and yield.

The invention relates to the technical field of organic synthesis and the technical field of fluorescent materials, in particular to a boron coordination salicylhydrazone double-state emission fluorophore as well as a preparation method and application of the boron coordination salicylhydrazone double-state emission fluorophore. The structure of the boron coordination salicylazone double-state emission fluorophore is shown as I, II or III; wherein R1 is selected from one of H, halogen atoms, diethylamino and thienyl, R2 is selected from one of H, halogen atoms, diethylamino and thienyl, and R3 is selected from one of aryl, 9, 9 '-spirobifluorenyl, alkoxy and halogen atoms. The boron coordination salicylazone double-state emission fluorophore is diversified in structure and good in solubility, has excellent photophysical properties and extremely high quantum yield, and also shows excellent biocompatibility and remarkable liposome targeting property at the same time. Moreover, the preparation method of the boron-coordinated salicylazone double-state emission fluorophore adopts a one-pot two-step method, is simple and convenient, is high in yield, is green and environment-friendly, and has a wide application prospect.

The invention discloses a method for continuously synthesizing long-chain alkyl modified silicone oil, which belongs to the technical field of organic synthesis, and comprises the following specific steps: quickly mixing hydrogen-containing silicone oil and long-chain olefin in a micro-mixer, carrying out hydrosilylation reaction in a packed tubular reactor, controlling the reaction residence time by using the tube length, and continuously synthesizing the long-chain alkyl modified silicone oil. Controlling the material ratio by utilizing the reaction liquid flow ratio, controlling the reaction temperature by utilizing a water bath, and obtaining a mixed solution containing modified silicone oil after the reaction is completed; and decoloring the mixed solution by using activated carbon, and then carrying out reduced pressure rotary evaporation on the decolored mixed solution to finally obtain a modified silicone oil pure product. The method realizes continuous synthesis of the modified silicone oil, and has the advantages of simple process, short reaction time and high reaction safety.

The invention relates to a synthesis method of a diunsaturated ester compound catalyzed by N-heterocyclic carbene, and belongs to the field of organic synthesis. According to the preparation method, the synergistic effect of N-heterocyclic carbene and light is utilized, gamma-oxo unsaturated aldehyde and Katritzky salt are taken as starting raw materials, the Katritzky salt generates alpha-ester free radicals through a single electron transfer process under the illumination condition, the free radicals react with a nucleophilic trienol intermediate generated through catalysis of the N-heterocyclic carbene, and the alpha-ester free radicals react with the nucleophilic trienol intermediate to generate the gamma-oxo unsaturated aldehyde. Target products are obtained with good yield and high regioselectivity, so that a series of epsilon-alkylated diunsaturated ester compounds are efficiently synthesized. The method is simple and convenient to operate, green and efficient, has the advantages of no transition metal participation, wide substrate applicability and the like, provides a new way for synthesis of the diunsaturated ester compound, and has a wide application prospect.

The invention belongs to the technical field of organic synthesis, and particularly relates to a salicylaldehyde hydrazone bridged organic boron photoinitiator as well as a preparation method and application thereof. The structural formula of the salicylaldehyde hydrazone bridged organic boron photoinitiator is as shown in formula I, wherein R is H or halogen atom; the salicylaldehyde hydrazone bridged organic boron photoinitiator has a vertical spatial configuration formed by a seven-membered ring and a six-membered ring. A framework of the salicylaldehyde hydrazone bridged organic boron photoinitiator has a unique vertical spatial configuration, generation of a spinning triplet state can be effectively promoted through orbital angular momentum regulation and control, and a more favorable excited state characteristic is provided for a photoinitiation process. The absorption wavelength and the emission spectrum of an LED light source are well overlapped, and high reaction activity can still be kept under the conditions of low irradiation intensity (lt, 60 mW / cm) and short exposure time (lt, 60 s). In addition, the preparation method of the salicylaldehyde hydrazone bridged organic boron photoinitiator is simple and efficient, the raw material cost is low, and the salicylaldehyde hydrazone bridged organic boron photoinitiator has a wide application prospect.

The invention relates to a preparation method of triethylene glycol diacetate, and belongs to the technical field of organic synthesis. The method comprises the following steps: adding triethylene glycol, an acetylation reagent and a multifunctional catalyst into a reaction kettle provided with a stirrer, a thermometer and a reflux condensing tube, and stirring and heating for reaction under the protection of nitrogen; after the reaction is finished, cooling reaction liquid to room temperature, and filtering and recovering the catalyst; performing reduced pressure distillation and silica gel column purification on the filtered reaction liquid to obtain triethylene glycol diacetate; the multifunctional catalyst is prepared from mesoporous silicon dioxide microspheres, 3-mercaptopropyltrimethoxysilane, 4-vinyl benzo-18-crown ether, sodium ethoxide, absolute ethyl alcohol, an ethanol solution of tetrabutyl titanate and chlorosulfonic acid. The preparation method comprises the following steps: preparing the mesoporous silicon dioxide microspheres, 3-mercaptopropyltrimethoxysilane, 4-vinyl benzo-18-crown ether, sodium ethoxide, absolute ethyl alcohol, the ethanol solution of tetrabutyl titanate and chlorosulfonic acid; the triethylene glycol diacetate prepared by the method has high yield and high purity, and can meet industrial production and market requirements.

The invention discloses a precise construction strategy of a dibenzothiophene sulfuryl covalent organic framework material and systematically explains efficient application of the dibenzothiophene sulfuryl covalent organic framework material in photocatalytic synthesis of thiadiazole and derivatives thereof. The achievement relates to a plurality of leading subjects such as catalytic chemistry, organic synthesis, material science, environmental engineering and green chemistry. According to the method, 2, 4, 6-triformyl phloroglucinol and 3, 7-diaminodibenzo [b, d] thiophene-5, 5-dioxide are taken as construction units, and the crystalline S-COF rich in sulfuryl active sites can be quantitatively obtained through topology-oriented Schiff base condensation under the conditions of protonic acid catalysis, no water and no oxygen. Under the radiation condition of visible blue light, S-COF is used as a heterogeneous photocatalyst to drive green synthesis of 3, 5-di-p-tolyl-1, 2, 4-thiadiazole and series of derivatives thereof; the invention provides a new catalyst design normal form for light-induced organic conversion, and lays a solid foundation for sustainable development-oriented efficient synthesis chemistry.

The invention belongs to the technical field of fine chemical organic synthesis, and discloses a synthesis method of 1, 3-propane sultone without generation of three wastes. The synthesis method comprises the following steps: by taking allyl alcohol, sulfite and hydrosulfite as raw materials, generating 3-hydroxy propanesulfonate; then removing part of water, adding a solvent A to separate out sulfite, filtering, and adding sulfuric acid into filtrate for acidification; and adding a solvent B to separate out sulfate, filtering and separating out the sulfate, and adding a dehydrating agent to carry out dehydration cyclization reaction to prepare the 1, 3-propane sultone. According to the synthesis method provided by the invention, a 1, 3-propane sultone product with the yield not lower than 95% and the purity reaching 99.9% or above and a sulfate byproduct with the purity reaching 99.6% or above can be obtained; no waste gas, waste solid or waste water is generated in the reaction process, the catalyst sulfite can be repeatedly used, and the used solvent is easy to recover and can be repeatedly used.

The invention relates to the technical field of organic synthesis, in particular to a method for constructing Orforglipron tetrahydropyran ring chirality through enzyme catalysis, which comprises the following steps: step S1, taking SM1 as a raw material, and carrying out hydrolysis resolution in a solvent, a buffer salt system and enzyme catalysis to obtain a chiral pure intermediate INT-1; step S2; performing ring closing on the INT-1 through Grignard reaction to synthesize a lactone intermediate; s3, carrying out Diball-H reduction, quenching, dichloromethane extraction and anhydrous sodium sulfate drying on the INT-4, and then reducing the INT-4 by using triethyl silane to obtain an intermediate INT3; step S4, coupling the INT-3 in the presence of a catalyst and a ligand to obtain an intermediate INT-4; step S5, carrying out deprotection and salification on the INT-4 to obtain an intermediate INT5; s6, closing an indole ring from INT5 to obtain a compound of which the general formula is A; chirality is constructed through enzyme catalysis, isomer impurities do not need to be split and separated through SFC when the chirality is constructed, the loss is reduced, the yield is increased, and a target product is obtained with high chiral selectivity; meanwhile, the cost is relatively reduced, and the cost is saved.

The invention belongs to the technical field of organic synthesis, and relates to a preparation method of 5, 5-dimethyl-4, 5-dihydroisoxazole. The method comprises the following steps: (1) reacting isopentenal with an oximation agent to obtain a reaction solution containing isopentenal oxime; (2) dropwise adding the reaction liquid into a mixture containing isopentenal and an acid catalyst for reaction to obtain a product; or when the reaction liquid contains water, performing phase splitting on the reaction liquid to obtain an organic phase, and dropwise adding the organic phase into a mixture containing the isopentenal and the acid catalyst for reaction to obtain a product. The method does not produce ketone by-products, and is good in atom economy, high in reaction yield, good in technological process continuity, low in cost, few in materials, simple to operate, mild in reaction condition, low in requirements on production equipment and suitable for large-scale industrial production.

The invention belongs to the technical field of organic synthesis, and particularly relates to a pyroxasulfone preparation method which specifically comprises the following steps: dissolving 3-(5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5, 5-dimethyl-2-isoxazoline serving as a raw material with a solvent, then adding a boron compound, finally dropwise adding hydrogen peroxide, and reacting at room temperature to obtain the pyroxasulfone. Reacting for several hours to obtain pyroxasulfone; the adopted boron compound is cheap and easy to obtain, so that the use of a transition metal catalyst is avoided, and the raw material cost is reduced; organic acid reagents with heavy odor are not used, waste water and solid waste are less, and the method has great advantages in the aspect of environmental protection; the method is simple to operate, free of complex treatment steps and suitable for industrial production, and when the boron compound is selected from sodium metaborate, sodium perborate or a mixture of borax and sodium metaborate, the yield and purity of the process are higher, and sulfoxide impurities are fewer.

The present invention discloses a method for preparing a pinaverium bromide intermediate having a high content of cis isomers, relating to the technical field of organic synthesis. By introducing an acidic chiral reagent into the system, the content of compound III isomer is significantly increased, and the trans isomer content is controlled to ≤2.0%, thus having advantages for industrial production.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of butynedioic acid. The preparation method of the butynedioic acid comprises the following steps that butynediol is oxidized into the butynedioic acid through pypocholoride and a catalyst, and the catalyst comprises carbon black and a metal compound loaded on the carbon black. According to the invention, butynediol is used as a raw material, and butynediol is oxidized by using pypocholoride and a catalyst to prepare butynedioic acid. Wherein butynediol is easy to obtain, and the raw material cost is low. In addition, the catalyst uses carbon black to immobilize a metal compound, conversion of pypocholoride into a large number of reactive oxygen free radicals can be accelerated, butynediol can be efficiently oxidized under the action of pypocholoride and the catalyst, and the whole synthesis route is safe and green, simple and feasible in process, low in equipment requirement, low in operation cost, free of secondary pollution and low in production cost.

The invention relates to the technical field of organic synthetic chemistry, in particular to a preparation method of ethyl 2-n-butyl acetoacetate, which comprises the following specific steps: S1, preparation of a composite solid base catalyst, S2, synthesis of ethyl 2-n-butyl acetoacetate, S3, post-treatment of a reaction solution, and S4, separation and purification of a product. The preparation method has the following beneficial effects that the magnesium-aluminum composite oxide is used as a carrier, and the composite solid base catalyst loaded with potassium and lanthanum has relatively high catalytic activity and selectivity; the magnesium-aluminum composite oxide carrier has a relatively large specific surface area and rich alkaline sites, so that a good catalytic environment is provided for the reaction; as a main active component, potassium ions can effectively activate alpha-active methylene of ethyl acetoacetate and promote formation of negative ion intermediates; the introduction of lanthanum ions can adjust the electronic structure of the catalyst, enhance the stability of the active center and inhibit the occurrence of side reactions.

The invention provides an organic synthesis steam recovery device, and relates to the technical field of steam recovery, the organic synthesis steam recovery device comprises a steam recovery tank and a built-in air flotation separation tank, a spiral cold water pipe and a spiral partition plate are arranged in the steam recovery tank, and an organic matter separation pipe and a gas overflow port with a gas diffusion plate are arranged in the air flotation separation tank; steam enters from the steam inlet and then is subjected to reverse convection condensation along the spiral partition plate and the spiral cold water pipe, condensate water and uncondensed gas enter the air flotation separation tank after being subjected to bubble refining through the gas dispersing plate, and organic matter impurities are separated from pure condensate water through the secondary condensation and air flotation effects in the bubble rising process. The device solves the problems of insufficient condensation, difficult impurity separation and loose structure, has the advantages of thorough heat energy recovery, accurate organic matter separation and stable and compact operation, and is suitable for efficient treatment and resource recycling of high-temperature impurity-containing steam in the organic synthesis industry.