4140 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 method of bromo-pyrrole nitrile. The method comprises the following steps: (1) mixing p-chlorophenylglycine, acetonitrile, trifluoroacetic acid and a catalyst, then dropwise adding acyl chloride and carrying out acylation reaction, and after the reaction is completed, purging with an inert gas; (2) under the inert gas, mixing the mixture obtained in the step (1) with inorganic salt, then dropwise adding 2-chloroacrylonitrile, carrying out cyclization reaction, and separating a liquid phase from the obtained mixture; and (3) under the inert gas, mixing the liquid phase obtained in the step (2), hydrobromic acid and hydrogen peroxide, carrying out a bromination reaction, then extracting with acetonitrile to obtain an acetonitrile layer, then removing the acetonitrile, and then carrying out cooling crystallization to obtain the bromo-pyrrolenitrile. According to the technical scheme, the reaction yield is high, different solvents do not need to be frequently replaced, and the solvents can be recycled.

The invention discloses a carbon fiber surface treatment process, which belongs to the technical field of organic synthesis, and comprises the following steps: S1, taking melamine, adding into tetrahydrofuran, adding carboxylated carbon fiber and a condensing agent, heating to 50-60 DEG C, stirring for 3-4 hours, washing, and drying to obtain melamine modified carbon fiber; s2, adding nano silicon dioxide into DMF (Dimethyl Formamide), performing ultrasonic treatment, adding a silane coupling agent KH550 and succinic anhydride, stirring for 3-5 hours, washing and drying to obtain modified silicon dioxide; and S3, adding the modified silicon dioxide into DMF, adding the melamine modified carbon fiber and a condensing agent, heating to 90-100 DEG C, stirring for 4-5 hours, washing, and drying to obtain the surface-treated carbon fiber. The silane coupling agent KH550 and butanedioic anhydride are used for carboxylation modification of nano silicon dioxide, melamine is used as a coupling agent, nano silicon dioxide is grafted on carbon fibers, surface defects on the surfaces of the carbon fibers can be filled, and therefore the mechanical performance of the carbon fibers is improved.

The invention discloses a composite water purifying agent based on polyaluminum ferric sulfate. The preparation process comprises the following steps: 1, reacting ferrous sulfate heptahydrate, aluminum sulfate, sodium chlorate, phosphoric acid and the like to prepare a polyaluminum ferric sulfate solution; 2, mixing the modified polyacrylamide solution with the polyaluminum ferric sulfate solution for reaction to obtain a composite system; and step 3, adding acidic ochre soil into the composite system to obtain the composite water purifying agent. The preparation method has the beneficial effects that a modified monomer is prepared through organic synthesis, and the modified monomer is copolymerized with monomers such as acrylamide to prepare modified polyacrylamide; then, the organic polymer is compounded with a polyaluminum ferric sulfate solution and acidic ochre soil, and an inorganic-organic-mineral ternary water purification system is constructed; the composite water purifying agent has the high-efficiency electricity neutralization capability of an inorganic flocculating agent, the bridging flocculation effect of organic macromolecules and the adsorption performance of minerals, and shows excellent flocculation and sedimentation effects and pollutant removal capability.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of p-tert-butoxystyrene. According to the preparation method provided by the invention, the p-tert-butoxystyrene is prepared by utilizing the continuous flow microreactor, the operation is simple and safe, the efficiency is high, the reaction time is short, the temperature is low, expensive reagents are not used, the amplification effect does not exist, the prepared p-tert-butoxystyrene product is high in yield and purity and stable in quality, and the method is suitable for large-scale production and has wide application prospects. The production cost can be greatly reduced, and the production safety is improved.

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 preparation method of 4-bromo-2-(4-chlorphenyl)-5-trifluoromethyl-1H-pyrrole-3-formonitrile, and belongs to the technical field of organic synthesis.The preparation method comprises the steps of acylation reaction, cyclization reaction, bromination reaction and recovery. The preparation method disclosed by the invention is high in safety, the prepared 4-bromo-2-(4-chlorphenyl)-5-trifluoromethyl-1H-pyrrole-3-formonitrile is high in purity and yield, the equipment investment is small, the bromination reaction speed is high, the acid-binding agent can be recycled, the drying time during recycling is short, and the water content in the recycled acid-binding agent is low.

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.

The invention discloses a preparation method of hydrogenated benvitimod and analogues thereof, and belongs to the technical field of organic synthesis. The method comprises the following steps: S1, mixing a compound I and palladium carbon in a solvent to obtain slurry; s2, under the protection of nitrogen, preheating the silicon carbide microchannel reactor to 20-70 DEG C, and then introducing hydrogen and the slurry in the step S1; the reaction temperature is 20-70 DEG C, the reaction pressure is 1-10 kg, and the retention time of the slurry is 1-20 min; and S3, carrying out solid-liquid separation, concentration, recrystallization and drying on the reaction liquid in the step S2 to obtain a compound II. The method adopts continuous flow production and is suitable for industrial production; the reaction speed is high, and the residence time does not exceed 20 min and is much shorter than overnight time in the prior art; the reaction yield is high and can reach 95% or above, and the yield of part of compounds can reach 99% or above; the catalyst dosage is small, and the reaction cost is greatly reduced.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of ethylene sulfate and derivatives thereof, which comprises the following steps: S1, taking an aprotic solvent as a reaction solvent, adding urea peroxide, and stirring until the urea peroxide is dissolved; s2, dropwise adding ethylene sulfite or an ethylene sulfite derivative, stirring for reaction, and purifying to obtain ethylene sulfate or an ethylene sulfate derivative; the method has the advantages of reducing the catalyst cost and reducing the wastewater amount.

The invention relates to the field of organic synthesis, and discloses a continuous deuteration preparation method of perdeuterated carbazole. The method comprises the following steps: taking carbazole and a deuterium source as raw materials, reacting under the catalysis conditions of a solvent and a catalyst, collecting an effluent reaction solution, cooling, filtering, concentrating and recrystallizing to obtain the perdeuterated carbazole. According to the present invention, the heavy metal chloride is adopted to catalyze the continuous reaction, the carbazole is adopted as the raw material, the hydrogen-deuterium exchange with the deuterium source is performed to synthesize the perdeuterated carbazole, the reaction condition is mild, the deuterium source is supplemented for multiple times during the reaction process so as to achieve the continuous deuteration, and the conversion rate and the yield are substantially improved. The whole reaction system is carried out in an isolated environment, no other impurities enter the reaction system, the product is free of pollution in the production process, the yield reaches 91% or above, the purity reaches 99.8% or above, and the deuteration degree reaches 99% or above. The whole process does not need high-temperature and high-pressure conditions, is relatively simple and convenient to operate, and facilitates 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 provides a process method for preparing (2-(3, 6-dimethoxy-9H-carbazole-9-yl) ethyl) phosphonic acid, and particularly relates to the technical field of organic synthesis. The process method comprises the following steps: under an alkaline condition, adding a halogenated phosphonate compound into a 3, 6-dimethoxy-9H-carbazole solution for reaction, after the reaction is finished, adding a hydrochloric acid aqueous solution for acidolysis degreasing, and finally extracting, refluxing, adsorbing, pulping and purifying to obtain the (2-(3, 6-dimethoxy-9H-carbazole-9-yl) ethyl) phosphonic acid. According to the process method, 3, 6-dimethoxy-9H-carbazole is adopted as a starting material, synthesis of a target product is achieved through a one-pot reaction, reaction conditions are mild, used raw materials are non-toxic and easy to obtain, the synthesis process is simple, operation is convenient and fast, and the separation yield is high.

The invention discloses a preparation method of pyridinetriazolone, and belongs to the technical field of organic synthesis, and the preparation method comprises the following steps: taking hydrazine hydrate as a starting raw material, adding urea in batches at the temperature of 80-85 DEG C, carrying out heat preservation reaction to obtain semicarbazide, dropwise adding hydrochloric acid to form salt, and drying under reduced pressure to obtain semicarbazide hydrochloride; adding the semicarbazide hydrochloride obtained in the previous step and 2-chloropyridine into an ethylene glycol monomethyl ether system, heating to 130-135 DEG C, refluxing, adding a catalytic amount of concentrated sulfuric acid, and carrying out heat preservation reaction to obtain pyridine triazolone; and drying the post-treated mother liquor under reduced pressure, weighing, adding quantitative urea, heating to 130-135 DEG C, and reacting to obtain the pyridinium triazolone. The initial raw materials are hydrazine hydrate and urea, are common industrial raw materials, are easy to obtain and low in price, and are beneficial to industrial production; the by-product 2-hydrazinopyridine is recovered and reacts with urea to prepare the pyridintriazolone, so that the raw material utilization rate and the product yield are greatly improved, the total yield reaches more than 80%, and the purity of the pyridintriazolone is more than or equal to 99.0%.

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 provides organic silicon cooling liquid and a preparation method thereof. The molecular structural formula of the organic silicon cooling liquid is shown in the specification, R1 is selected from C3-7alkane, the value of a is 0-12, and the value of b is 14-20. A phenyl group and a long-chain alkyl side chain are introduced into a silicone oil main chain through an organic synthesis means, the regularity of a polysiloxane chain is destroyed, the crystallization property of the polysiloxane chain is reduced, the performance of the organic silicon cooling liquid is changed from the molecular structure, and the organic silicon cooling liquid can still flow at a low temperature (-65 DEG C). In addition, by introducing phenyl, the flash point, irradiation resistance and other properties of the immersed cooling liquid can be remarkably improved. # imgabs0 #

The invention provides a plate-type micro-channel reactor and a method for nitrifying trifluoromethoxybenzene by using the plate-type micro-channel reactor, and belongs to the technical field of organic synthesis. The plate type microchannel reactor comprises a first heat exchange plate, a reaction plate and a second heat exchange plate, the reaction plate is positioned between the first heat exchange plate and the second heat exchange plate; a feeding channel, a first shunting section, a first mixing section, a second shunting mixing section, a third shunting mixing section, a fourth shunting mixing section and a discharging channel which are connected in sequence are arranged on the reaction plate; and the feeding channel comprises a first feeding channel and a second feeding channel. According to the method, trifluoromethoxybenzene is taken as a raw material and is subjected to nitration reaction by using plate type micro-channel reactors connected in series, so that high-selectivity continuous nitration of trifluoromethoxybenzene is realized, the nitration reaction can be completed within 5 minutes, and the contents of byproduct meta-position and dinitrate can be controlled to be lower than 0.05% and 0.5% respectively.

The invention belongs to the technical field of organic synthesis of ethers, and particularly relates to a method for continuously synthesizing ethylene glycol dimethyl ether. The method comprises the following steps that ethylene glycol, sodium hydroxide and methane chloride serve as raw materials, multi-stage continuous reaction is carried out in liquid membrane reactors to synthesize ethylene glycol dimethyl ether, ethylene glycol, sodium hydroxide and methane chloride are introduced into the first-stage liquid membrane reactor, sodium hydroxide and methane chloride are introduced into the subsequent stages of liquid membrane reactors, and the first-stage liquid membrane reactor and the second-stage liquid membrane reactor are connected with the second-stage liquid membrane reactor. A byproduct sodium chloride is separated from a reaction product in the previous-stage liquid membrane reactor and then enters the next-stage liquid membrane reactor, a byproduct sodium chloride is separated from a reaction product in the last-stage liquid membrane reactor and then clear liquid is obtained, and ethylene glycol dimethyl ether is obtained through rectification treatment. The invention develops a novel process mode for continuously synthesizing an ethylene glycol dimethyl ether product, and provides a new idea for large-scale continuous production of ethylene glycol dimethyl ether.

The invention relates to the technical field of organic synthesis, in particular to a synthesis method and application of functional caprolactam and functional nylon-6. The synthesis method comprises the following steps: in the presence of a catalyst and a solvent, enabling amino caprolactam and / or a derivative thereof to contact and react with benzaldehyde, so as to obtain functional caprolactam which is bis (benzyl) amino caprolactam, wherein the reaction conditions are as follows: the temperature is 150-350 DEG C; the hydrogen pressure is 0.1 to 10 MPa; the time is 5-15 hours. The synthesis method not only has the advantages of high reaction efficiency, high catalytic efficiency, adjustable target product selectivity and the like, but also simplifies process conditions, and realizes green large-scale production.

The invention relates to the technical field of organic synthesis, in particular to a method for homogeneous catalytic synthesis of dimethyl carbonate by using a liquid separation method to separate a catalyst, which comprises the following steps: by using 0.3-15% long-chain tertiary amine as a homogeneous catalyst, carrying out homogeneous reaction on cyclic carbonate and methanol in a mass ratio of 1: (1.2-5.5) at 60-80 DEG C for 4-7 hours. And after the homogeneous transesterification reaction is completed, carrying out atmospheric distillation on the reaction mixture, and collecting fractions to obtain the target product dimethyl carbonate. Carrying out liquid separation on the heterogeneous atmospheric distillation residual liquid, and collecting a lower-layer material to obtain a by-product; and the collected material is a catalyst which can be directly recycled subsequently. The dimethyl carbonate synthesis method provided by the invention has the characteristics of high catalytic efficiency, easy catalyst separation, environmental protection, energy saving and the like.

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 relates to the technical field of textile, in particular to a xylitol-containing plant-source composite ultra-short fiber and a preparation method thereof.The xylitol-containing plant-source composite ultra-short fiber comprises an ultra-short fiber base material and plant-source functional particles, the plant-source functional particles are obtained by conducting chemical modification, microencapsulation and nanocrystallization treatment on citramalic acid, xylitol and plant-source extracts, and the plant-source functional particles are prepared from the ultra-short fiber base material and the plant-source extracts. According to the present invention, the heat absorption characteristic of xylitol is utilized to achieve the contact cool feeling effect, the antibacterial components of the plant source extract are adopted to form the antibacterial barrier so as to prevent the growth and the reproduction of bacteria and achieve the antibacterial effect, and the stability of the functional components is significantly enhanced through the chemical modification of citramalic acid; microencapsulation and nanocrystallization treatment improve the dispersibility and compatibility of the plant-derived functional particles in fibers and ensure more lasting and effective functional performance, and meanwhile, the components of the plant-derived functional particles are all derived from the nature and have the characteristics of reproducibility and degradability, so that the plant-derived functional particles can effectively replace traditional organic synthesis functional modification aids.

The invention discloses a mechanical force-induced fluorescence discoloration sensor material as well as a preparation method and application thereof, and relates to the technical field of organic synthesis and fine chemical engineering. The preparation method comprises the following steps: step 1, carrying out heating reaction on 4-(1, 2, 2-triphenyl vinyl) benzaldehyde, 3-(2, 2-dicyano-1-(3, 4-diaminophenyl) vinyl) benzene-1-yl and a catalyst to prepare a compound 1-1; and 2, carrying out heating reaction on the obtained compound 1-1 and methyl iodide under the action of alkali and a solvent, and analyzing and purifying to obtain a compound 1-2. The compound disclosed by the invention is low in preparation cost, simple and convenient to operate and simple in method, the compound shows the material characteristic of mechanical force-induced fluorescence discoloration and can be applied to the fields of sensors, dyes, anti-counterfeiting and the like, and meanwhile, the synthesis method can be used for synthesis in the fields of fine organic chemical engineering such as luminescent materials, printing and dyeing technologies and the like.

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 present invention relates to a fluxapyroxad intermediate trifluoronitrobiphenyl synthesis method, and belongs to the technical field of organic synthesis, the method comprises the following steps: Step 1: under nitrogen protection, adding 3, 4, 5-bromotrifluorobenzene, o-nitrophenylboronic acid, a catalyst, a promoter, an alkali and a solvent into a reaction flask, and after addition, carrying out a heat preservation reaction; and Step 2: after the reaction is finished, carrying out phase splitting and organic phase concentration to obtain the 3 ', 4', 5 '-trifluoro-2-nitrobiphenyl. Compared with a traditional synthetic method of the trifluoro-nitrobiphenyl, the synthetic method of the trifluoro-nitrobiphenyl has the advantages that the 3, 4, 5-trifluoro-bromobenzene and the o-nitrophenylboronic acid are directly used as raw materials, the production step of preparing the 3, 4, 5-trifluoro-phenylboronic acid from the 3, 4, 5-trifluoro-bromobenzene through a multi-step reaction is avoided, the yield can be effectively improved, the utilization rate of the raw materials is high, and the method is suitable for industrial production. And the o-nitrophenylboronic acid preparation method is simple, the reaction cost can be effectively reduced, the reaction route is shorter, simpler and more efficient, the reaction conditions are mild, and the method has higher industrial application value.

The present invention relates to the technical field of organic synthesis, particularly to a daphnetin preparation method, which comprises: adopting 2, 3, 4-trihydroxybenzaldehyde and Meldrum's acid as starting raw materials, and carrying out a first-step reaction under the action of a first catalyst to obtain an intermediate 7, 8-dihydroxycoumarin-3-carboxylic acid; the intermediate 7, 8-dihydroxycoumarin-3-carboxylic acid is subjected to a second-step reaction under the action of a second catalyst, and daphnetin is obtained. The method has the remarkable advantages that firstly, the reaction process is easy to control, the generation amount of byproducts is low, and the product is excellent in appearance quality and extremely high in purity; and secondly, the use of chemicals with high risk and high toxicity is avoided, meanwhile, a large amount of acid waste liquid is not generated, and the environmental pollution is effectively reduced. In addition, the recycling of the solvent and the catalyst further reduces the production cost. The yield and the purity are remarkably improved, the total yield can reach 90% or above, the purity exceeds 99%, and the method is very suitable for industrial large-scale production.

The invention provides a pyrrolidone dihydroisoxazole compound as well as a preparation method and application thereof, and belongs to the technical field of organic synthesis. Specifically, under the catalytic action of Lewis base, beta-oxoacrylamide and 4-nitroisoxazole serve as raw materials, and the pyrrolidone dihydroisoxazole compound is synthesized through a one-step method. Beta-oxoacrylamide and 4-nitroisoxazole which are simple and easy to obtain are adopted as starting raw materials, dearomatization [3 + 2]-cycloaddition reaction is carried out under the catalysis of Lewis base, the pyrrolidone dihydroisoxazole compound is synthesized, the method is easy and convenient to operate and mild in reaction condition, the used reagents and raw materials are economical and easy to obtain, and the method is suitable for industrial production. The target product yield is high, the substrate application range is wide, and the in-vitro anti-tumor activity is good.

The invention discloses an allyl pentafluorosulfenyl compound as well as a preparation method and application thereof, and belongs to the technical field of organic synthesis. The structural formula of the allyl pentafluorosulfenyl compound is as follows: # imgabs0 #. The preparation method comprises the following steps: by taking an allyl compound and a pentafluorothio source as raw materials, carrying out an allylpentafluorothio reaction in a solvent under the induction of visible light to obtain the allylpentafluorothio compound by a one-step method, so that the reaction time is extremely short, the conversion of a substrate can be completed within only 15 seconds, the reaction conditions are mild, and the yield is high. The reaction can be completed under sunlight, and the allyl pentafluorosulfenyl compound derivative drug molecule has biological activity and shows a certain anticancer effect.

The invention discloses a radioactive labeling method of [18F] trifluoromethyl terminal olefin in the technical field of organic synthesis, under the condition of room temperature, 3, 3-difluoroallyl sulfosalt is used as a precursor, [18F] KF / K222 or [18F] TBAF is used as a fluorinating reagent, acetonitrile is used as a solvent, very high radiochemical yield can be obtained within 30 seconds, the tolerance of functional groups is excellent, and the method is suitable for industrial production. The specific reaction formula is as follows: # imgabs0 #. The method provides a simple and efficient way for producing the [18F] trifluoromethylated terminal olefin compound, so that the [18F] trifluoromethylated terminal olefin compound can be applied to positron emission tomography imaging. According to the method for preparing the 3, 3-difluoroallyl sulfur salt compound, the raw materials are easy to obtain, the cost is low, the operation is simple and convenient, safety and controllability are realized, and the radiation yield of the obtained product is high.

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.