2220 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 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 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 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 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 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 belongs to the technical field of organic synthesis, and provides a preparation method of a cationic lipid compound, which comprises the following steps: (1) reacting 1, 5-dihalopentane, 2-tert-butyl glycolate and alkali to obtain a product G; (2) hydrolyzing the product G under an acidic condition to obtain a product H; (3) carrying out esterification reaction on the product H, the raw material C, 4-dimethylaminopyridine and a condensing agent in dichloromethane to obtain a product J; and (4) carrying out amination reaction on the product J, the raw material L and alkali in acetonitrile to obtain the cationic lipid compound. Compared with the prior art, the method has the relatively remarkable advantages that when the first part of halogenated long-chain alkyl ester H is synthesized by the method, 1, 5-dihalopentane and 2-tert-butyl glycolate are used as raw materials, the halogenated long-chain alkyl ester J is synthesized by a simple method, the product is obtained at a higher yield in synthesis, and the method is suitable for kilogram-level production. The route synthesis only comprises four steps of chemical reactions, and is suitable for industrial production.

The invention belongs to the technical field of organic synthesis, and particularly relates to an alkyl pentafluorosulfenyl compound and a preparation method and application thereof.The preparation method comprises the following steps that in the protective gas atmosphere, in a solvent, SF5Cl serves as a pentafluorosulfenyl source, an olefin compound serves as a reaction substrate and a free radical trapping agent, a thiol compound serves as a hydrogen source, and the alkyl pentafluorosulfenyl compound is obtained through a one-step reaction; under the action of an olefin additive, the alkyl pentafluorothio compound is constructed by a one-step method through a visible light-induced free radical process, and the olefin additive is used for inhibiting generation of a pentafluorothio chloride byproduct from a pentafluorothio source and an olefin compound. According to the method disclosed by the invention, a series of alkyl pentafluorosulfenyl compounds can be prepared by only needing olefin double bonds in substrates and selecting more substrates through the reaction, the reaction is simple, the reaction condition is mild, the reaction can be completed under visible light, the reaction time is short, the implementation is easy, and the method is suitable for industrial production. And a method support is provided for further screening the alkyl pentafluorosulfenyl compound with excellent biological activity.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of N, N '-dichloro-1, 4-benzenedicarboxamide, which comprises the following steps: taking terephthalamide as an initial raw material and tert-butyl hypochlorite as a chlorination reagent; the method comprises the following steps: carrying out a chlorination reaction on terephthalamide and tert-butyl hypochlorite in a solvent under the protection of inert gas by controlling the reaction temperature, and after the reaction is finished, carrying out post-treatment to obtain N, N-dichloro-1, 4-phthalimide. The preparation method of the N, N '-dichloro-1, 4-benzenedicarboxamide comprises the following steps: taking terephthalamide and tert-butyl hypochlorite as raw materials, and carrying out one-step reaction to generate a dichloro product. Compared with a traditional N, N '-dichloro-1, 4-benzenedicarboxamide production method, the preparation method has the advantages that the amount of three wastes generated is small, the product yield is high, the product purity is high, the operation is safe and convenient, and the preparation method is more suitable for industrial application.

The invention provides a preparation method of 2-pentyl-2-cyclopentenone, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: carrying out a first-stage isomerization reaction on 2-pentylidene cyclopentanone and a first composite catalyst in a first atmosphere to obtain an intermediate, carrying out a second-stage isomerization reaction on the intermediate and a second composite catalyst in a second atmosphere, and controlling the volume ratio of nitrogen to hydrogen in the first atmosphere and the second atmosphere to obtain the 2-pentylidene cyclopentanone. In the first-stage isomerization reaction, the conversion rate of converting 2-pentylidene cyclopentanone into 2-pentyl-2-cyclopentenone is increased, and in the second-stage isomerization reaction, the use amount of hydrogen in the second atmosphere is reduced, the temperature of the second-stage isomerization reaction is increased, generation of by-products is inhibited, and the yield of 2-pentylidene cyclopentanone is increased. Further, the yield and the purity of the 2-pentyl-2-cyclopentenone can be improved. According to the preparation method, the first-stage isomerization reaction and the second-stage isomerization reaction are continuous reactions, intermittent reactions are not needed, and the preparation method is more suitable for industrial application.

The present invention relates to the technical field of organic synthesis, and specifically relates to a method for constructing the chirality of a pyran ring in Orforglipron by means of enzymatic catalysis, the method comprising the following steps: step S1, by using SM1 and SM2 as starting materials, carrying out a reaction under the action of a palladium catalyst and a ligand to obtain INT-1; step S2, under the catalysis of Pd / C, subjecting INT-1 to double bond hydrogenation reduction to obtain INT-2; step S3, in the presence of a solvent, a buffer salt system and enzymatic catalysis, subjecting INT-2 to hydrolysis and resolution to obtain a chirally pure intermediate INT-3; step S4, subjecting INT-3 to a Grignard reaction for cyclization, so as to synthesize a lactone intermediate INT-4; and step S5, subjecting INT-4 to reduction by means of Dibal-H, quenching same, performing extraction with dichloromethane, drying same with anhydrous sodium sulfate, and then performing reduction by means of triethylsilane to obtain a compound of general formula A. In the present invention, the chirality is constructed by means of enzymatic catalysis without the need of SFC resolution for separating isomeric impurities during the construction of the chirality, thereby reducing losses and improving yield, obtaining the target product at high yield and high chiral selectivity, and further saving expenses and reducing costs.

The invention belongs to the field of organic synthesis, and discloses an aldol condensation reaction method and a catalyst thereof.The method comprises the steps that in the presence of a composite catalyst, a substrate 1 and a substrate 2 are subjected to an aldol condensation reaction, after the reaction is finished, an aldol condensation product is collected from reaction products, according to the method, aldol condensation reaction of fatty aldehyde or aromatic aldehyde is catalyzed by adopting the novel composite catalyst, and the method has the advantages of being mild in reaction condition, environmentally friendly, efficient and simple in post-treatment.

The invention relates to the technical field of organic synthesis, in particular to 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine as well as a synthesis method and application of the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine. The synthesis method comprises the following steps: (1) synthesizing 2-chloro-3-fluoro-4-iodine-5-methylpyridine from 2-chloro-3-fluoro-5-methylpyridine and an iodine elementary substance to obtain 2-chloro-3-fluoro-4-iodine-5-methylpyridine; (2) synthesizing 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine, the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride, the tripotassium phosphate and the (2-formyl phenyl) boric acid, and further synthesizing the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine and the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride. And (3) synthesizing the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine by using the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde and sodium tert-butoxide. The 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine compound constructed by the invention can be used for detecting the content of pesticide residue glyphosate.

The invention belongs to the technical field of organic synthesis, and particularly relates to a catalyst-free continuous production method of chlorotert-butane, which comprises the following steps: adding diluted hydrochloric acid as a starting solution into the tower kettle of a reactive distillation tower, and heating the tower kettle to boil until reflux exists at the tower top; the method comprises the following steps: adding tert-butyl alcohol and concentrated hydrochloric acid into a mixing preheater for preheating, then continuously feeding from a feed port of a reactive distillation tower until the tower top temperature is 45-48 DEG C, the side discharge port temperature is 50-52 DEG C and the tower kettle temperature is 96-105 DEG C, and carrying out reflux according to a reflux ratio of (1.5-3): 1; and continuously extracting crude chlorinated tert-butane from a side discharge port of the tower, cooling, neutralizing, drying and filtering to obtain the chlorinated tert-butane. According to the invention, through the integrated design of the mixing preheater and the reactive distillation column, especially by utilizing the reactive distillation technology to continuously remove the product, the chemical equilibrium limitation of the traditional intermittent process is successfully broken, the raw material conversion rate is obviously improved, and meanwhile, the green production targets of flow simplification, energy consumption reduction and three-waste emission reduction are realized.

The invention belongs to the technical field of organic synthesis, and provides a preparation method of isobutyric anhydride. The preparation method provided by the invention comprises the following steps: by taking isobutyric acid as a raw material and TiO2, gamma-Al2O3, SiO2, CuO, palladium-loaded silicon dioxide or triethyl phosphate as a catalyst, dehydrating to form isobutyric anhydride; the catalyst does not react with isobutyric acid, so that side reactions are few in the reaction process, the conversion rate of isobutyric acid and the selectivity of isobutyric anhydride are improved, and finally the yield of isobutyric anhydride is improved. Meanwhile, isobutyric anhydride can be separated from isobutyric acid and water through simple condensation, high-purity isobutyric anhydride is obtained, and continuous production can be achieved.

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazole compound under a visible light catalysis condition. The method comprises the following steps: dissolving a compound 1 in 1, 2-dichloroethane, then adding tert-butyl nitrite, tribromomethane, alkali and a photocatalyst, in an inert gas environment, irradiating with visible light and stirring at room temperature to react, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column purification on a crude product to obtain a product, namely the isoxazole compound. The brand-new method for preparing the isoxazole compound through visible light catalysis is developed, the conditions of high temperature and high pressure in a traditional synthesis method are avoided, energy consumption and environmental pollution are remarkably reduced, and the yield of the isoxazole compound is effectively increased by regulating and controlling reaction conditions and optimizing raw material selection and proportion.

The invention belongs to the technical field of organic synthetic chemistry and pesticide science, and particularly relates to an indole-containing amide derivative as well as a preparation method and application thereof, and the indole-containing amide derivative has a structure as shown in a formula I or a formula II, through an active substructure splicing strategy, indole is used as a parent skeleton, amido bonds are ingeniously introduced for structural diversity optimization and modification, active functional groups such as methoxyamine are further introduced, and a series of indole amide derivatives with novel structures are designed and synthesized. Through determination, the screened series of compounds show good antibacterial activity, and a plurality of compounds show excellent prevention and treatment effects on various important crop diseases.

The invention belongs to the technical field of organic synthesis, and particularly relates to a process for catalytically synthesizing ascorbyl tetraisopalmitate by a biological enzyme. The synthesis process comprises the following steps: attaching a biological enzyme to a metal organic framework compound material (MOFs material) to prepare biological enzyme catalyst powder, and adding a small amount of biological enzyme catalyst powder into methyl n-hexylcaprate and ascorbic acid which are used as raw materials for transesterification to prepare ascorbyl tetraisopalmitate. The process route is simple, few three wastes are generated, compared with a traditional preparation process of tetra-isopalm ascorbate, the yield and purity of the product are greatly improved, and experimental results show that the highest yield of the product is 89%, and the purity of the product reaches 99.0%.