122 results about "Dichloroethane" patented technology

The invention relates to a preparation method of a lithium difluoro bis (oxalate) phosphate concentrated solution, and belongs to the technical field of lithium battery electrolyte additives. Adding lithium oxalate into a solvent, stirring and dissolving to obtain a lithium oxalate solution; the method comprises the following steps: adding a modified fluorine ion chelating agent into a lithium oxalate solution, stirring, filtering, putting into a reactor, and slowly introducing phosphorus pentafluoride gas; after the introduction is finished, heating and stirring for reaction; after the reaction is finished, filtering reaction liquid to remove unreacted solid impurities, so as to obtain a lithium difluoro bis (oxalate) phosphate concentrated solution; the modified fluorine ion chelating agent is prepared from D301 ion exchange resin, dichloroethane, propylene-1-base boronic acid pinacol ester, mercaptoethyl guanidine dihydro bromide and sodium tert-butoxide. The lithium difluoro bis (oxalate) phosphate prepared by the method is high in purity and high in yield, and meets the use requirements of lithium ion battery electrolyte on lithium salt.

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 discloses a Pd-Ba / C catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps: step 1, pretreating a carbon carrier; step 2, preparing a complexing solution containing a barium complex; step 3, carrying out wet impregnation to obtain a carbon carrier adsorbed with a barium complex; 4, performing low-temperature pyrolysis to obtain a barium pre-modified carrier; 5, a complexing solution containing palladium and barium complexes is prepared; step 6, co-adsorption of bimetals is realized through wet impregnation, and a bimetal adsorption carrier is obtained; step 7, freeze drying; 8, the precursor obtained after freeze drying is subjected to hydrogen reduction, and the Pd-Ba / C catalyst is obtained. The invention provides application of the Pd-Ba / C catalyst in preparation of ethylene by hydrodechlorination of 1, 2-dichloroethane. According to the invention, pre-loaded barium occupies a strong adsorption site on the surface of the activated carbon, so that the stability and dispersity of a palladium active center can be enhanced, and synergistic improvement of chlorine poisoning resistance and catalytic performance of the catalyst is realized.

The invention belongs to the technical field of synthesis of organic compounds, and particularly relates to a process for preparing fipronil and an intermediate thereof. Toxic 1, 2-dichloroethane is comprehensively replaced by bio-based gamma-valerolactone, low-toxicity cyclopentyl methyl ether is matched, and N, N-dimethylformamide necessary for the process is recycled, so that consumption is greatly reduced; the continuous processes of amination, diazotization and the like are realized through a tubular reactor, a micro-reactor and a static mixer, and separation technologies such as pervaporation membrane and vacuum distillation are combined, so that the reaction time is shortened, the solvent recovery rate is increased, and the production is promoted to be continuously transformed to green. The supported FeCl3 / SiO2-NH2 catalyst disclosed by the invention can be repeatedly used, and byproducts and tail gas can be recycled and reused. In addition, diazonium salt residues are controlled to be smaller than or equal to 0.5% through near infrared spectroscopy, citric acid is subjected to stable oxidation reaction, a purification process is combined, it is ensured that the finished product is high in purity, excellent in yield and small in batch fluctuation, and efficiency and safety are both considered.

The invention relates to the field of chemical equipment, in particular to a 1-nitroanthraquinone continuous production process based on a dynamic liquid membrane continuous flow reactor, which comprises a solid feeding device, a homogeneous emulsifier, a quenching kettle, a solid-liquid separator, a centrifugal separator and a dynamic liquid membrane reactor, a sulfuric acid storage tank is divided into two branches through a sulfuric acid feeding pump, one branch is connected to the dynamic liquid membrane reactor, the other branch is connected to the dynamic liquid membrane reactor through a flow self-control valve, the quenching kettle is connected to a solid-liquid separator, the solid-liquid separator is divided into two branches, one branch is connected to an anthraquinone crude product storage tank, the other branch is connected to a centrifugal separator, and the other branch is connected to a gas-liquid separator. The centrifugal separator is divided into two branches, one branch is connected to the acid water storage tank, and the other branch is connected to the dichloroethane storage tank, so that the reaction selectivity of the anthraquinone nitration reaction can be effectively improved, high-viscosity solids are prevented from being blocked, and the conversion rate of raw materials in the continuous reaction of the anthraquinone nitration reaction is improved.

The subject of the invention is N-substituted derivatives of l-(l-phenyl-3-aryl)-lH-pyrazol-4-yl)methanamine with the general formula 1, where ¥ represents CH or N, R1 represents hydrogen, R2 represents no substituent, R3 represents hydrogen, while R4 represents N-propylbenzamide, benzo[b]furan, dihydrobenzo [b] furan, methylenedioxybenzene, ethyl benzoate, or propyl benzoate, substituted accordingly, their method of production and application, and the method of obtaining and application of N-substituted derivatives of l-(l-phenyl-3-aryl)-IH-pyrazol-4-yl)methanamine with the general formula 1, where Y represents C, CH, or N, R1 represents hydrogen or a methyl group, R2 represents a methyl group or no substituent, R3 represents hydrogen or a methyl group, while R4 represents dimethylpyrazole, methylpyrazole, dimethylimidazo[l,2-a]pyrimidine, or isopropoxybenzene, substituted accordingly. The compounds that are the subject of the invention are obtained through reductive amination using borohydride derivatives as the reducing agent, advantageously sodium triacetoxyborohydride, in the amount of 1.4-2.0 eq, amine in the amount of 1.0-1.1 eq, advantageously in slight excess, base, advantageously triethylamine in the amount of 1.0-1.1 eq (in the case of using amine in the form of hydrochloride), and the starting aldehyde. The reaction is conducted in a nonpolar solvent environment, advantageously dichloroethane at a concentration of about 0.1 M. The crude product is purified by column chromatography on silica gel using a methanol in dichloromethane mixture as the eluent, in concentration ranges from 2% to 5%. In order to obtain a solid form and improve the physicochemical parameters, the free bases are converted into hydrochloride form, and then crystallized from a polar solvent, advantageously ethanol or propanol.

A macroporous cation exchange resin and its preparation and application method are disclosed. The method involves dispersing polystyrene-divinylbenzene microspheres in dichloroethane to obtain a microsphere suspension. A sulfonating agent, a mixture of fuming sulfuric acid and chlorosulfonic acid, is then slowly added dropwise under cooling and stirring conditions. After the addition is complete, heating is initiated to trigger a polysulfonation reaction. Once the reaction is complete, the reaction mixture is slowly poured into ice water and continuously stirred and diluted until the solution pH reaches 2.5. The solution is then filtered, washed, and dried to obtain a solid resin. This invention simultaneously introduces a matched number of sulfonic acid groups and sulfone groups onto the polystyrene-divinylbenzene backbone. Utilizing the electron-withdrawing effect of the sulfone groups and the rigid framework they form, the stability of the C-H and C-S bonds in the resin is enhanced. This solves the problems of resin structure damage, rapid decline in separation performance, and significantly shortened service life associated with existing cation exchange resins used in treating chromium plating aging solutions.

The application discloses a preparation method of 1-(2-aminoethyl) pyrrolidine and belongs to the field of chemical synthesis. The application provides a novel synthesis method of 1-(2-aminoethyl) pyrrolidine, which is prepared from 1,2-dichloroethane and pyrrolidine as raw materials, addition of a solvent and alkali, heating reaction, extraction, acidification and reduced-pressure distillation after the reaction is finished to obtain N-(2-chloroethyl) pyrrolidine solution; N-(2-chloroethyl) pyrrolidine and ammonia water are used as raw materials, high-pressure heating reaction is carried out, extraction and reduced-pressure distillation are carried out after the reaction is finished to generate 1-(2-aminoethyl) pyrrolidine. The application has the advantages of simple operation process, green process synthesis, convenient product purification and high product purity.

The invention discloses a method for preparing vinyl chloride by electrocatalytic dechlorination of 1, 2-dichloroethane, a working electrode of the method takes a metal oxide as a catalyst, and the metal oxide is selected from at least one of the following metal oxides: Pd, Mn, Fe, Co, Ni, Cu, Ru and Mo. According to the invention, the metal oxide powder is used as the electrocatalyst, the catalyst is coated on the electrode material to prepare the working electrode, the working electrode is applied to electrocatalytic dechlorination reaction of 1, 2-dichloroethane, vinyl chloride can be generated at high selectivity at room temperature, a new way is opened up for production of vinyl chloride by electrocatalytic dechlorination, and the method has wide application prospect. And a green and low-cost solution is provided for efficient synthesis of vinyl chloride.

The invention discloses amido-modified hypercrosslinked resin, a preparation method thereof and application of the amido-modified hypercrosslinked resin to adsorption of chlorine-containing VOCs (Volatile Organic Compounds). The preparation method comprises the following steps: chloromethylation: swelling hypercrosslinked NDA-88 resin in 1, 2-dichloroethane, adding anhydrous FeCl3 as a catalyst, and carrying out chloromethylation reaction at 35-40 DEG C to obtain chloromethylated resin; and amination: mixing the chloromethylated resin with an amination reagent diethylenetriamine, carrying out amination reaction at 140-150 DEG C, and carrying out post-treatment to obtain the amino modified hypercrosslinked resin. The amino-modified hypercrosslinked resin has high adsorption capacity and long penetration time for chlorine-containing VOCs (Volatile Organic Compounds) such as dichloromethane, chlorobenzene and the like, is stable in performance under the relative humidity of 50%, and is small in adsorption performance attenuation after multiple times of thermal regeneration. The resin is simple in preparation method, excellent in performance and suitable for efficient purification treatment of industrial chlorine-containing VOCs waste gas.

The invention discloses a method for preparing p-trifluoromethoxyphenol by adopting a micro-channel reactor, and belongs to the field of fine chemical engineering. 4-trifluoromethoxyaniline and dilute sulphuric acid are pumped into the first micro-channel reactor for a reaction; then introducing inert gas, pumping the nitroso sulfuric acid solution, and carrying out diazotization reaction to obtain a diazonium salt solution; pumping the diazonium salt solution into a second micro-channel reactor, carrying out hydrolysis reaction, adding dichloroethane extract liquor into a rectifying tower after the reaction is ended, and rectifying to obtain p-trifluoromethoxyphenol; porous baffles which are inclined downwards are arranged on the inner wall of the rectifying tower in a crossed manner; a heat-conducting filler layer of 50-100 nm is arranged on the porous baffle plate; the heat-conducting filler layer is a three-dimensional net-shaped material layer which is formed by boron nitride nanosheets / titanium oxide nanorods and has a porous structure. The method is simple in process route, convenient to operate, high in controllability, high in safety, high in reaction efficiency, high in product yield, capable of effectively reducing the solid waste amount in production, energy-saving, environment-friendly and suitable for industrial production.

This invention discloses a highly selective method for preparing triethylenetetramine. The method uses 2-chloroethylamine hydrochloride and ethylenediamine as raw materials, reacting them in an aqueous solution. An aqueous solution of ethylenediamine with a concentration of 1-100 wt% is added dropwise to an aqueous solution of 2-chloroethylamine hydrochloride with a concentration of 1-100 wt%. The dropping rate of the ethylenediamine solution is 5% to 100% of its own mass per hour. The reaction temperature is 30-200 °C (oil bath temperature), and the reaction time is 2-20 hours (including the dropping time). The molar ratio of 2-chloroethylamine hydrochloride to ethylenediamine is 2:1 to 40:1. This invention is the first to propose a direct synthesis of triethylenetetramine from the bulk chemicals 2-chloroethylamine hydrochloride and ethylenediamine. Compared with the previously reported dichloroethane amination method and the nucleophilic substitution method between dichloroethane and ethylenediamine, this method offers milder reaction conditions, simpler operation, and higher selectivity, making it suitable for industrial production.

The invention belongs to the technical field of polysulfide sealants, and relates to a bi-component modified polysulfide sealant for a binding surface as well as a preparation method and application of the bi-component modified polysulfide sealant. The bi-component modified polysulfide sealant for the binding surface is prepared from a component A and a component B according to the mass ratio of 100: (8-12), the component A comprises modified polysulfide rubber, a functional filler, a coupling agent, an adhesive and a regulator; the modified polysulfide rubber is prepared from polysulfide rubber and a modifier; the modifying agent is one of bis (2-chloroethyl) ether, 1, 2-dichloroethane and bis (chloromethyl) dimethylsilane; and the component B comprises a metal oxide, a plasticizer, an accelerant and a regulator. According to the modified polysulfide sealant formed by two components, the elongation at break of the polysulfide sealant is improved in an extreme environment, the sealant has excellent deformation resistance, cracking, shrinkage and bonding failure of a sealant layer are avoided, and the sealing performance of a binding surface is improved.

The utility model relates to the technical field of synthetic reaction devices of 2, 6-difluorobenzamide, in particular to a synthetic reaction device of 2, 6-difluorobenzamide, which comprises a stirring mechanism, the stirring mechanism comprises a supporting frame, a fixed bearing is fixedly arranged at the bottom end of the supporting frame, a stirring rod is fixedly arranged at the bottom end of the fixed bearing, a metal fixing sleeve is fixedly arranged on one side of the stirring rod, and a stirring paddle is fixedly arranged on one side of the metal fixing sleeve. And a supporting rotating platform is fixedly arranged at the bottom end of the stirring rod. Production materials are fed into the reaction kettle mechanism through the convenient feeding nozzle, then the stirring paddle is started by controlling the electric driving mechanism, and the stirring rod is controlled by the driving motor to rotate, so that the stirring paddle on one side of the stirring rod is driven to rotate and stir, the mixing of the coating is promoted, and the mixed 2, 4-dichloroethane is added into the reaction kettle mechanism. And 2, 6-difluorobenzamide is discharged through a discharge valve at the bottom of the reaction kettle mechanism and is conveyed to the next process.

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane, which comprises the following steps: by taking aromatic aldehyde, [1.1. 1] propeller alkane and 4-alkyl substituted Hanss ester synthesized by aldehyde as initial raw materials and dichloroethane and the like as a solvent, carrying out a reaction under the protection of inert gas to obtain 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane, and separating the 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane from the 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane. A three-component free radical coupling reaction is carried out under the illumination condition, and a 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane product is synthesized in one step. The method has the advantages of mild reaction conditions, high reaction efficiency, low cost, simplicity and convenience in operation and the like, and a new method is provided for later structural modification of diaryl methanol drug molecules.

The invention discloses a high-boiling-point styryl liquid cross-linking agent, a preparation method thereof and organic medium slurry of a high-frequency and high-speed copper-clad plate. The preparation method of the high-boiling-point styryl liquid cross-linking agent comprises the following steps: carrying out Friedel-Crafts reaction on toluene and dichloroethane to obtain 1, 2-bis (methyl benzene) ethane; the preparation method comprises the following steps: carrying out Friedel-Crafts reaction on dimethyl phenylethane and acetyl chloride to obtain 1, 2-bis (methyl acetyl benzene) ethane; the preparation method comprises the following steps: carrying out reduction reaction on 1, 2-bis (methyl acetyl benzene) ethane and sodium borohydride to obtain 1, 2-bis (methyl alpha hydroxyethyl benzene) ethane; and carrying out dehydration to obtain the 1, 2-bis (methyl vinyl benzene) ethane cross-linking agent. The 1, 2-bis (methyl vinyl benzene) ethane is in a liquid state at normal temperature, has high solubility for SEBS and other film-forming resins, can reduce the solvent amount for copper-clad plate manufacturing, is a high-boiling-point cross-linking agent, and has wide application prospects.

The invention discloses a preparation method of tris (2-cyanoethyl) phosphate, which comprises the following steps of: 1, adding 3-hydroxypropionitrile, an organic alkali acid-binding agent and a reaction organic solvent which is one of dichloromethane and dichloroethane into a reaction container, and reacting at the temperature of between 20 and 30 DEG C for 1 to 3 hours; controlling the temperature not to exceed 20 DEG C, dropwise adding a mixture formed by phosphorus trichloride and a reaction organic solvent, after dropwise adding is completed, performing heating reflux reaction, and after the reaction is completed, performing suction filtration to remove generated organic alkali hydrochloride so as to obtain filtrate; and 2, controlling the temperature of the filtrate obtained in the step 1 at 30-40 DEG C, introducing oxygen for reaction until the reaction is finished, and removing the reaction organic solvent to obtain the final product tris (2-cyanoethyl) phosphate. The method has the advantages of simplicity in operation, mild and controllable reaction, high product purity and suitability for industrial popularization.

The utility model provides a kettle for dehydration and alcohol removal of dichloroethane, which comprises a reaction kettle, the reaction kettle comprises a kettle body, a stirring mechanism is fixedly arranged at the top of the kettle body, a stirring shaft is fixedly connected with a transmission mechanism through a support rod, the bottom of the transmission mechanism is fixedly connected with a mixing mechanism, the mixing mechanism comprises a connecting seat, a stirring rod and a hydraulic cylinder, the connecting seat is fixedly connected with the bottom of the enclosure, the top end of the stirring rod is rotatably connected with the interior of the connecting seat, and a plurality of uniformly distributed rod bodies are arranged on the stirring rod. The stirring mechanism and the mixing mechanism are arranged in the kettle body and are matched to realize full mixing, and the mixing mechanism can be folded after stirring, so that the mixing efficiency can be improved, the subsequent standing layering cannot be influenced, the production period of dichloroethane can be effectively shortened, the production efficiency is improved, and the production cost is reduced. The dichloroethane recovery solvent is subjected to washing alcohol removal treatment, and the yield of acylation reaction is better stabilized and improved, so that the solvent scrap consumption and the production cost are reduced.

The invention relates to a device and a method for producing partially chlorinated alkanes by means of a direct chlorination of alkenes. In particular, the invention relates to a device and a method for producing 1,2-dichloroethane by means of a direct chlorination of ethene (synonym: ethylene). The invention is characterized in that a loop reactor is used for the direct chlorination, wherein the outlet for the produced partially chlorinated alkane is provided on a vertical position of the loop reactor (in the operating state) on a lateral wall of the loop reactor, the vertical position being situated below half the height of the loop reactor.

The application provides a synthesis method of 9,10-dibromoanthracene, by introducing HBr generated by a solvent water adsorption reaction, using an industrial sodium hypochlorite solution to react the HBr into bromine, ensuring high concentration of bromine, introducing a solvent dichloroethane to uniformly disperse raw materials, keeping the concentration of bromine stable in the reaction, greatly promoting the reaction speed, greatly shortening the reaction time, and converting the sodium hypochlorite into a sodium chloride aqueous solution after the reaction is completed. The purity of the prepared 9,10-dibromoanthracene is more than 99%, and the by-products generated in the reaction are environment-friendly and non-polluting.

The application belongs to the technical field of ion detection, and particularly relates to a preparation method of a rapid detection uranyl ion ratio type fluorescent probe, comprising the following steps: dissolving rhodamine B and phosphorus oxychloride in 1,2-dichloroethane to obtain product 1; dissolving the product 1 in acetonitrile, adding 2-aminobenzimidazole and triethylamine, and stirring under heating; after the reaction is completed, column chromatography purification is carried out, and vacuum drying is carried out to obtain the target product fluorescent probe RBN; and the fluorescent probe RBN is dissolved in DMSO to prepare a mother liquor. The fluorescent probe has the advantages of rapid response to uranyl ions, simple synthesis route, simple detection equipment and method, and the like, and can be used for qualitative and quantitative detection of uranyl ions in an environment and a biological system.

The invention discloses a preparation method and a preparation system of p-chloro-o-cresol, and the preparation method comprises the following steps: 1) adding dichloroethane into molten o-cresol, and adding a catalyst; (2) controlling the temperature to be 5-15 DEG C, and adding sulfuryl chloride into the material in the step (1) at different feeding speeds according to the reaction time and the reaction stage; and (3) after the reaction is finished, rectifying and purifying liquid of reaction materials to obtain the p-chloro-o-cresol. According to the present invention, the process is simple, the reaction condition is mild, the reaction is controlled, the selectivity is high, the ortho-cresol is subjected to preferential para-position chlorination, the reaction is sufficient, the selectivity is high, the polychlorination phenomenon is avoided, the phenol content and the isomer content in the crude product are low, the yield is high, and the large-scale production is easily achieved.

The invention belongs to the technical field of organic synthesis, and discloses a preparation method for trifluoromethylation of a 1, 6-enyne substrate. The preparation method comprises the following steps: in a protective gas atmosphere, mixing a 1, 6-eneyne substrate, NaSO2CF3, an oxidant, N-bromosuccinimide and an organic solvent, heating to react, cooling, separating an organic phase, drying and purifying to obtain a product after trifluoromethylation of the 1, 6-eneyne substrate, the organic solvent is selected from any one of dimethoxyethane and 1, 2-dichloroethane. The preparation method is mild in reaction condition, simple and convenient to operate, good in substrate applicability, good in substrate selectivity in reaction and high in target product yield, and a new way is provided for trifluoromethylation of the 1, 6-eneyne compound.

The utility model discloses a dichloroethane dehydration system and belongs to the technical field of rectification and purification. According to the technical scheme, the dichloroethane dehydration system comprises a refined dichloroethane cooler, a dehydration tower feeding / discharging heat exchanger, a dehydration tower, a dehydration tower top condenser, a mixer, a dehydration tower top reflux tank and a controller, an inlet of the dehydrating tower feeding / discharging heat exchanger is connected with a wet dichloroethane feeding pipeline, the wet dichloroethane feeding pipeline is provided with a first flow transmitter and a first flow adjusting valve, an outlet of the dehydrating tower feeding / discharging heat exchanger is connected with the dehydrating tower through a pipeline, and the bottom of the dehydrating tower is connected with a dehydrating tower bottom reboiler. The bottom of the dehydrating tower is also connected with a refined dichloroethane discharging pipeline; and the refined dichloroethane discharging pipeline is provided with a dehydrating tower bottom discharging pump, a refined dichloroethane cooler, a discharging regulating valve, a flow transmitter II and a water analyzer. The device has the advantages of high separation effect, continuous, stable and reliable operation and obvious economic effect.

The invention relates to a method for preparing a high-purity lithium difluoro (oxalato) borate solid through a low-temperature melting method, and belongs to the technical field of lithium battery electrolyte additives. The preparation method comprises the following steps: under the protection of argon, adding lithium oxalate, boric acid and lithium fluoride into a reaction kettle, uniformly stirring and mixing, and carrying out a low-temperature melting reaction to form a molten reaction product; naturally cooling the molten reaction product to room temperature, cooling and crystallizing, and separating out solid crystals; washing the solid crystals with absolute ethyl alcohol, performing centrifugal separation, and removing surface impurities through a modified resin adsorbent; drying the washed solid crystals in a vacuum drying oven to obtain a high-purity lithium difluoro (oxalato) borate solid; the modified resin adsorbent is prepared from styrene-divinylbenzene copolymer resin, dichloroethane, allyl phosphine dichloride, benzoyl peroxide and tetraallyl silicate. The lithium difluoro (oxalato) borate prepared by the method is high in purity and high in yield, and meets the use requirements of a high-energy-density lithium ion battery electrolyte.

This invention discloses an aminoindole derivative-based porous polymer, its preparation method, and its application, belonging to the field of dye adsorbent technology. The preparation method is as follows: 2-phenylindole is dissolved in acetic acid, and sodium nitrite aqueous solution is added dropwise. The system is then stirred and reacted at low temperature. After the reaction, the precipitate is collected and dried to obtain product 1. Product 1 is dissolved in ethanol, and NaOH solution is slowly added dropwise while stirring and mixing. Na2S2O4 is added, and the reaction is stirred under heating conditions. After the reaction, the precipitate is collected and dried to obtain product 2. Product 2, 1,2-dichloroethane, and dimethoxymethane are stirred and mixed. A catalyst is added, and the reaction is stirred and reacted under heating conditions. After the reaction, the precipitate is collected, washed, and dried to obtain the final product. The aminoindole derivative-based porous polymer of this application has high specific surface area, high adsorption rate, and high adsorption capacity, effectively solving the problems existing in the prior art.

The invention discloses a preparation method of an oral PCSK9 inhibitor cyclopeptide drug, and belongs to the technical field of medicinal chemistry. The preparation method comprises the following steps: sequentially coupling Fmoc amino acids or polypeptide fragments on alpha-Me-Pro-CTC resin by adopting a solid-phase synthesis method until peptide resin is obtained, then treating with a cutting liquid, adding 1, 2-dichloroethane and a Zhan catalyst 1B to carry out a ring-closure reaction, adding a Pd / C catalyst, and carrying out a hydrogenation reaction under the protection of hydrogen, so as to obtain the Fmoc peptide. And then carrying out cyclization reaction under the action of a condensing agent, and after the reaction is finished, carrying out purification treatment to obtain the oral PCSK9 inhibitor cyclopeptide medicine. A fragment synthesis strategy is adopted, the synthesis path is remarkably shortened, and the problems of low yield and difficult purification in traditional step-by-step synthesis are effectively solved; meanwhile, by optimizing reaction conditions, the reaction efficiency and selectivity are improved, the difficulty and risk of amplified production are greatly reduced, and a reliable synthesis route is provided for industrial production of a target product.

The invention relates to a device and process for recycling triethylamine in 4.6-dichloro-5-fluoropyrimidine production. The device comprises a reaction kettle, a filter press, a neutralization kettle, a distillation kettle and a receiving tank, and triethylamine acid salt solids output by a triethylamine tank are leached by dichloroethane in the reaction kettle; the discharging end of the reaction kettle is connected with the feeding end of the filter press, the solid material output end of the filter press is connected with the feeding end of the neutralization kettle, the feeding end of the neutralization kettle is further connected with the alkali liquor tank, and the discharging end of the neutralization kettle is connected with a water phase receiving tank and an organic phase receiving tank which are arranged in parallel. The output end of the organic receiving tank is connected with the input end of the distillation kettle; the input end of the receiving tank is connected with the upper end of the distillation kettle through a condenser, and gaseous triethylamine discharged from the distillation kettle enters the receiving tank after being cooled by the condenser. The method is reasonable in design, the production cost of 4.6-dichloro-5-fluoropyrimidine synthesis is effectively reduced, the amount of three wastes is reduced, the acid-binding agent triethylamine is recycled and reused, and meanwhile, the production environment for treating the catalyst in the production process is improved.

This invention provides a method for preparing green oxime ester, comprising the following steps: adding dichloroethane and m-trifluoromethylacetophenone oxime to a synthesis reactor, stirring until dissolved, then adding granular sodium hydroxide, stirring at 22℃-33℃ for 0.5h-2h, then adding potassium carbonate and tetrabutylammonium bromide, cooling, and then adding brominated oxime ether for a condensation reaction, adding water after the reaction and separating the layers, removing the lower oil phase under vacuum to remove dichloroethane, adding 90% methanol for crystallization, filtering, washing, and drying to obtain oxime ester. This invention uses dichloroethane throughout the condensation, bromination, and extraction steps, simplifying the solvent system and reducing residues and energy consumption; the combination of granular sodium hydroxide and potassium carbonate ensures efficient deprotonation and in-situ dehydration, suppressing side reactions and thus improving yield and purity; in the preparation of brominated oxime ether, n-butanol is recycled and crystallized in a controlled manner, achieving reduced consumption and safety, while saline wastewater is neutralized and recovered, effectively reducing chemical oxygen demand emissions.

The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a method for simultaneously extracting and purifying glabridin, glycyrrhizic acid and isoliquiritigenin by a column chromatography extraction method. The method comprises the following steps: adding an ethanol solution into glycyrrhiza glabra, extracting by adopting a column chromatography extraction method, extracting an extracting solution by using dichloroethane, enabling an organic phase to pass through a silica gel column, and crystallizing an eluent to obtain glabridin. Acidifying and centrifuging the extracted water phase, and dissolving the precipitate with acetone to obtain glycyrrhizic acid; and extracting and purifying the filtrate to obtain the isoliquiritigenin. The invention provides a simple and efficient new extraction technology which is low in energy consumption, small in solvent dosage and high in extraction rate compared with traditional ultrasonic extraction and the like, and aims to extract glycyrrhizic acid and glabridin in glycyrrhiza glabra at the same time, separate glycyrrhizic acid and glabridin, separate isoliquiritigenin from the remaining part through simple conversion, and improve the purity of glycyrrhizic acid and glabridin in glycyrrhiza glabra. The comprehensive development and utilization of the glycyrrhiza glabra are achieved.