24 results about "Ethyl bromoacetate" patented technology

The invention relates to the field of pipes, and discloses a high-flame-retardance MPP cable protection pipe and a preparation method thereof.The cable protection pipe comprises polypropylene resin, modified graphene oxide, modified maleic anhydride grafted polypropylene and auxiliaries; the modified graphene oxide is prepared by grafting a modified benzotriazole intermediate and a double-bond DOPO derivative substituted cyclotriphosphazene derivative into graphene oxide; the modified benzotriazole intermediate is prepared by grafting 2-(2, 4-dihydroxyphenyl)-2H-benzotriazole and ethyl bromoacetate, and then reacting with 2, 2, 6, 6-tetramethyl-4-piperidinol; the double-bond DOPO derivative is prepared through the reaction of DOPO-HQ and 4-vinyl benzyl chloride; the modified maleic anhydride grafted polypropylene is prepared by grafting octa-aminopropyl polyhedral oligomeric silsesquioxane prepared by a polycondensation reaction of 3-aminopropyltriethoxysilane and maleic anhydride grafted polypropylene. The pipe prepared by the invention has good mechanical properties, ultraviolet aging resistance, low-temperature toughness, heat resistance, flame retardance and wear resistance.

The present application relates to a kind of electrolyte additives and its preparation method, belong to electrolyte technical field;The present application uses propenyl-1,3-sulfonic acid lactone as raw material, using the double bond of propenyl-1,3-sulfonic acid lactone and the amino group of 4-amino-2-(trifluoromethyl) thiophene occurs Michael addition reaction under the catalysis of 1,8-diazabicyclo (7-ene) Undecane, obtain the intermediate with tertiary amine structure, then through the quaternary ammonium salt reaction of tertiary amine structure of intermediate and bromo atom of ethyl bromoacetate, obtain additive, the additive of the present application and phosphate ester additive are compounded to obtain electrolyte additive, the present application is modified by propenyl-1,3-sulfonic acid lactone, introduce fluorinated alkyl, effectively reduce intermolecular force, weaken the dependence of electrolyte viscosity on temperature, improve the ionic conductivity of electrolyte under low temperature condition.

The invention discloses a substituted benzoxazinone-isoxazoline compound as well as a preparation method and application of the substituted benzoxazinone-isoxazoline compound. The preparation method comprises the following steps: by taking DMF (Dimethyl Formamide) as a solvent, reacting ethyl bromoacetate with a compound (II) to generate a compound (III), performing cyclization in the presence of acetic acid and reduced iron powder to obtain a compound (IV), reacting the compound (IV) with hydroxylamine hydrochloride to generate a compound (V), reacting the compound (V) with NCS and MMA (Methyl Methacrylate) in the presence of TEA (Tetraethyl Ammonium) to generate a compound (VI), and reacting the compound (VI) with NCS and MMA to generate a compound (V). Reacting the compound (VI) with propargyl bromide to obtain a substituted benzoxazinone-isoxazoline compound, performing alkaline hydrolysis on the substituted benzoxazinone-isoxazoline compound, and performing condensation reaction on the substituted benzoxazinone-isoxazoline compound and alcohol or amine to obtain a target product. According to the present invention, the weeding activity test results of the obtained product show that the inhibition effects of the compounds I1, I2, I4, I15 and I16 on the rape are good under the concentration of 100 ppm, the excellent weeding activity is provided, and the good prevention and control effect on the invasive organism zinnia elegans is provided.

The invention relates to a synthesis method of (S)-2, 2, 4-trimethyl pyrrolidine hydrochloride, which comprises the following steps: step a, carrying out Michael addition reaction on a compound 10 and a compound 11 in the presence of a solvent to prepare a compound 12; b, the compound 12 and ethyl bromoacetate are subjected to an affinity substitution reaction under the alkaline and solvent conditions, and a compound 13 is prepared; c, carrying out condensation ring closing reaction on the compound 13 under alkaline and solvent conditions to prepare a compound 14; step d, the compound 14 is subjected to a decarboxylation reaction under the acidic condition, and a compound 15 is prepared; e, the compound 15 is subjected to Wittig reaction under the alkaline condition, and a compound 16 is prepared; and step f, carrying out asymmetric hydrogenation reaction on the compound 16 to prepare a target compound 1, namely (S)-2, 2, 4-trimethylpyrrolidine hydrochloride. According to the synthetic method of the (S)-2, 2, 4-trimethylpyrrolidine hydrochloride, the reaction type of the whole synthetic route is safe, the yield of each step is relatively high, and industrial production is convenient to realize.

The invention discloses an organic diphosphate ligand and a preparation method and application thereof, the structural formula of the ligand is shown in the specification, and the preparation method comprises the following steps: dissolving tetraethyl methylene diphosphate in an organic solvent, adding a catalyst and ethyl bromoacetate, and reacting to obtain an ethyl diphosphate intermediate; and reacting the diphosphate ethyl ester intermediate with acid to obtain the organic diphosphate ligand. The organic diphosphate ligand can efficiently chelate nuclide ions, can be used for removing nuclides contaminated on the body surface and can also promote discharge of nuclides in the body.

The invention relates to the field of high polymer materials, and discloses a modified nylon composition for door and window heat insulation strips and a preparation method thereof, the composition comprises nylon resin, modified glass fiber, modified nano titanium dioxide and an auxiliary agent; the modified glass fiber is prepared by grafting a functional additive on the surface of the glass fiber; the functional additive is prepared by replacing phosphonitrilic chloride trimer with a Schiff base product prepared by reaction of 4-hydroxy-2-trifluoromethyl benzaldehyde and 2-aminobenzimidazole and a modified silane coupling agent and reacting with DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide); the modified nano titanium dioxide is prepared by grafting a benzotriazole derivative and isocyanated nano titanium dioxide, wherein the benzotriazole derivative is prepared by taking 2-(2, 4-dihydroxyphenyl)-2H-benzotriazole, ethyl bromoacetate and tris (2-hydroxyethyl) isocyanurate as raw materials; the composition prepared by the invention has excellent tensile strength, ultraviolet aging resistance, hydrophobicity, heat resistance, antibacterial property and flame retardance.

This invention relates to the field of lithium battery technology, and more particularly to a preparation process for a lithium battery additive. The process first prepares a Zn-MOF-74 catalyst through dissolution, crystallization, separation, and stepwise vacuum drying. Then, using γ-valerolactone as a solvent, propenyl-1,3-sulfonyl lactone undergoes an addition reaction with 4-aminophenylboronic acid under the action of the catalyst to generate an intermediate. This intermediate then undergoes a substitution reaction with ethyl bromoethyl, followed by recrystallization and vacuum drying to obtain a sulfonate-boron-oxygen heterocyclic synergistic additive. This additive utilizes the synergistic effect of the sulfonate group and the boron-oxygen heterocycle to improve the ionic conductivity of the electrolyte and inhibit its decomposition, significantly improving the room-temperature cycle life, wide-temperature-range discharge performance, and high-temperature storage stability of lithium batteries. The preparation process is controllable, the product has high purity, and it is suitable for various high-performance lithium batteries.

The application discloses a preparation method of an intermediate N-methyl-2-hydroxyethyl pyrrolidine of clemastine, relates to the technical field of medicine intermediate synthesis, and comprises the following steps: triphenylphosphine is added into an organic solvent, ethyl bromoacetate is added, stirring reaction is carried out, filtration is carried out, the obtained precipitate is washed with the above-mentioned organic solvent, vacuum drying is carried out, and an intermediate one is obtained; N-methyl pyrrolidone is added into a benzene solvent, the intermediate one is added under stirring, stirring reaction is carried out, solid is removed through filtration, the filtrate is distilled under reduced pressure, and an intermediate two is obtained; the intermediate two is added into an alcohol solvent, hydrogenation is carried out through palladium-carbon, sodium borohydride is added in three batches, stirring reaction is carried out, pH is adjusted, extraction is carried out with dichloromethane, the obtained aqueous phase is extracted with dichloromethane again, organic phases are combined, drying is carried out, and N-methyl-2-hydroxyethyl pyrrolidine is obtained through reduced pressure distillation; the preparation method is high in yield, convenient in separation and purification, low in cost, simple and convenient to operate, and small in danger.

The invention relates to the field of filter bags, and discloses a PPS dust removal filter bag and a preparation method thereof, the dust removal filter bag comprises polyphenylene sulfide resin, a modified composite filler and a hyperbranched additive; the modified composite filler is prepared by grafting a modified silane coupling agent and the composite filler; according to the modified silane coupling agent, cyanuric chloride and an aminated antioxidant prepared through a reaction of 3-(3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl chloride and p-phenylenediamine are subjected to substitution to prepare a triazine ring substituent, and then N, N '-bis-(2, 2, 6, 6-tetramethyl-4-piperidyl)-1, 2, 4-triazine-1, 3, 5-triazine-1, 3, 5-triazine-1, 3, 5-triazine-1, 3, 5-triazine-1, 3, 5-triazine-1, 3-triazine-1, 3-triazine-1 the triazine ring intermediate is prepared by reacting 1, 6-hexamethylenediamine with a triazine ring substituent, and the triazine ring intermediate is grafted with 3-aminopropyltriethoxysilane. The hyperbranched additive is prepared by carrying out ester exchange on an additive intermediate prepared by reacting tris (2-hydroxyethyl) isocyanurate and ethyl bromoacetate and diphenyl dihydroxysilane. The material prepared by the invention has good mechanical properties, oxidation resistance, high temperature resistance, wear resistance and ultraviolet resistance.

The invention discloses a preparation method of an intermediate N-methyl-2-hydroxyethyl pyrrolidine for clomastine, and relates to the technical field of synthesis of medical intermediates, and the preparation method comprises the following steps: adding triphenylphosphine into an organic solvent, adding ethyl bromoacetate, stirring for reaction, filtering, washing the obtained precipitate with the organic solvent, and carrying out vacuum drying to obtain an intermediate I; adding N-methyl pyrrolidone into a benzene solvent, adding the intermediate I under stirring, carrying out stirring reaction, filtering to remove solids, and carrying out reduced pressure distillation on filtrate to obtain an intermediate II; adding the intermediate II into an alcohol solvent, carrying out palladium-carbon hydrogenation, adding sodium borohydride in three batches, carrying out a stirring reaction, adjusting the pH value, extracting with dichloromethane, extracting an obtained water phase with dichloromethane, combining organic phases, drying, and carrying out reduced pressure distillation to obtain N-methyl-2-hydroxyethyl pyrrolidine; the preparation method disclosed by the invention is high in yield, convenient to separate and purify, low in cost, simple and convenient to operate and low in risk.

The invention discloses a method and a device for synthesizing ethyl azidoacetate by a microchannel reactor, and belongs to the technical field of azide compounds. According to the technical scheme, the method for synthesizing ethyl azidoacetate through the micro-channel reactor comprises the following steps: taking one of ethyl chloroacetate and ethyl bromoacetate and sodium azide as initial raw materials, taking water as a reaction solvent, carrying out reaction by adopting the micro-channel reactor under a heating condition, and carrying out post-treatment to obtain ethyl azidoacetate, the adopted device comprises a micro-channel reactor and a controller, and the micro-channel reactor is provided with a first feed port, a second feed port and a discharge port; the microchannel reactor is provided with a plurality of reaction channels, each reaction channel comprises a plurality of mixing units, and each mixing unit is internally provided with a herringbone shunting structure and a streaming area. The method has the advantages of high reaction efficiency, high product yield, reduced solvent amount, simple post-treatment, production cost saving, and realization of efficient, safe and continuous synthesis of ethyl azidoacetate.

The invention discloses a preparation method of phentolamine EP impurity acid salt, which comprises the following steps: (1) taking a compound I resorcinol and a compound II p-toluidine as raw materials, and performing dehydration reaction to obtain an intermediate product III; (2) carrying out nucleophilic substitution reaction on the intermediate product III and benzyl bromide to generate an intermediate product IV; (3) carrying out nucleophilic substitution reaction on the intermediate product IV and ethyl bromoacetate to obtain an intermediate product V; (4) carrying out ester amidation reaction on the intermediate product V and N-tert-butyloxycarbonyl-1, 2-ethylenediamine to obtain an intermediate product VI; and (5) taking the intermediate product VI, and carrying out deprotection reaction to obtain a final product VII, wherein X represents hydrochloric acid, sulfuric acid, acetic acid, formic acid or trifluoroacetic acid. The purity of the prepared phentolamine EP impurity acid salt reaches 99% or above, the reaction yield is high, a test sample is provided for phentolamine research, and the phentolamine EP impurity acid salt has important research value in clinical pharmacokinetic research.

The invention provides an isoindolone-containing CDK4 / 6 inhibitor and a preparation method and application thereof.The preparation method comprises the steps that ethyl bromoacetate is introduced to a piperazine group of a palbociclib structure to be hydrolyzed into acid, then amido bonds are generated to be linked with different isoindolone, and a series of compounds shown in the formula I are synthesized; the compound can be used for preventing or treating mammalian diseases related to abnormal expression of CDK4 / 6 and anti-tumor, anti-virus, antibacterial and anti-inflammatory related to CDK4 / 6. I.

The invention relates to a preparation method of flurbiprofen axetil, and belongs to the technical field of medicine synthesis. In order to solve the problems of long synthetic route and low product yield in the prior art, the invention provides the flurbiprofen axetil preparation method, which comprises the following steps: in the presence of an acid-binding agent, carrying out alkylation reaction on ethyl 1-bromoacetate and 2-bromopropionic acid to obtain a compound shown as a formula IV; under the action of a coupling catalyst, a Grignard reagent and the compound shown in the formula IV are subjected to a coupling reaction, and the product flurbiprofen axetil is obtained. According to the method, the step of firstly synthesizing flurbiprofen ethyl ester and then hydrolyzing the flurbiprofen ethyl ester is not needed, the synthesis route is simplified, and the reduction of intermediate steps is beneficial to improving the yield and quality of the product.

The invention relates to the technical field of ion exchange membranes, and provides a preparation method of a 3D polymer nanochannel membrane for osmotic energy conversion, comprising: in a nitrogen environment, dissolving 1,4-dimethoxybenzene and paraformaldehyde in 1,2-dichloroethane, and then adding a first catalyst to react to obtain a first precipitate; dissolving the first precipitate in dichloromethane, and then adding a second catalyst to react to obtain a second precipitate; dissolving the second precipitate and potassium carbonate in acetonitrile, and then injecting ethyl bromoacetate to react to obtain a third precipitate; dissolving the third precipitate in tetrahydrofuran, and then adding a NaOH solution to react to obtain a fourth precipitate; dissolving the fourth precipitate, 2,5-diaminobenzenesulfonic acid, EDC and DMAP in DMF to react to obtain a fifth precipitate; dissolving sulfonated polyetheretherketone and the fifth precipitate in N,N-dimethylformamide to obtain a second liquid, and coating the second liquid on a stripping plate to obtain a channel membrane, so as to enhance the ion selectivity of the channel membrane.

The invention belongs to the technical field of chemical medicine preparation, and particularly relates to a preparation method of an omarigliflozin raw material. The raw material of the omariglitazone is 5-bromine-2-indole ethyl formate, and the preparation method comprises the following steps: firstly, under the action of an alkaline reagent, carrying out coupling reaction on 4-bromoaniline and ethyl chloroacetate or ethyl bromoacetate in an organic solvent to obtain a compound as shown in a structural formula I; then carrying out condensation reaction on the compound as shown in the structural formula I and N, N-dimethylformamide dimethyl acetal to obtain a compound as shown in a structural formula II; finally, under the action of lewis acid, the compound shown in the structural formula II is subjected to Friedel-Crafts reaction in an organic solvent, and a compound A is obtained. The method provided by the invention is simple to operate, the adopted raw materials are cheap and easy to obtain, and the cost is low; in the process, a large amount of acid does not need to be used, less acid waste is generated, the yield of each step is high, post-treatment is simple, and sustainable development in industrial production is facilitated.

The invention relates to an electrolyte additive and a preparation method thereof, and belongs to the technical field of electrolyte. The preparation method comprises the following steps: by taking allyl-1, 3-sultone as a raw material, carrying out Michael addition reaction on double bonds of the allyl-1, 3-sultone and amino groups of 4-amino-2-(trifluoromethyl) thiophene under the catalytic action of 1, 8-diazabicyclo-undec-7-ene to obtain an intermediate with a tertiary amine structure, and carrying out condensation reaction on the intermediate to obtain an intermediate with a tertiary amine structure; the preparation method comprises the following steps: carrying out a quaternary ammonium salt reaction on a tertiary amine structure of an intermediate and bromine atoms of ethyl bromoacetate to obtain an additive, and compounding the additive and a phosphate additive to obtain the electrolyte additive. Allyl-1, 3-sultone is used for modification, and fluoroalkyl is introduced, so that the intermolecular force is effectively reduced; the dependence of the electrolyte viscosity on the temperature is weakened, and the ionic conductivity of the electrolyte under the low-temperature condition is improved.

The invention discloses [1] rotaxane molecular compounds and a synthetic method thereof, and the synthetic method comprises the following steps: under the protection of inert atmosphere, carrying out nucleophilic substitution reaction on a compound A, sodium hydride and ethyl bromoacetate in N, N-dimethylformamide to obtain a compound B; performing nucleophilic substitution reaction with pyridine and trifluoromethanesulfonic anhydride to obtain a compound C; then carrying out a coupling substitution reaction with a compound D, bis (triphenylphosphine) palladium dichloride and 2-dicyclohexylphosphine-2 ', 4', 6 '-triisopropyl biphenyl to obtain a compound E; performing hydrolysis reaction with sodium hydroxide to obtain a compound F; under the protection of inert atmosphere, carrying out nucleophilic substitution reaction on the compound G, the compound H and potassium carbonate in N, N-dimethylformamide to obtain a compound I; performing hydrazinolysis reaction on the compound I and hydrazine hydrate to obtain a compound J; and under the protection of inert atmosphere, carrying out condensation reaction on the compound J, a compound F, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride and 1-hydroxybenzotriazole to obtain the [1] rotaxane molecular compound.

The invention discloses a synthesis method of cis-5-octylene-1-alcohol, and relates to the technical field of fine chemical engineering, and the synthesis method comprises the following steps: 1, taking leaf alcohol as an initial raw material, and carrying out substitution reaction with thionyl chloride to obtain 1-chloro-(Z)-3-hexene; 2, reacting 1-chloro-(Z)-3-hexene with magnesium chips to obtain a cis-3-hexene magnesium chloride Grignard reagent, and reacting the Grignard reagent with ethyl bromoacetate in the presence of a catalyst to obtain cis-5-ethyl octenate; and 3, carrying out a reduction reaction on the cis-5-ethyl octenoate and red aluminum, so as to obtain the cis-5-octylene-1-alcohol. The synthetic route is mild in reaction condition, low in cost and suitable for industrial production, and the total yield of the three steps can reach 72%.

The present invention provides a 4,4'-bipyridyl ester salt compound and its preparation method and application. The following steps are included: 4,4'-bipyridyl, compound 1 and compound 2 are respectively dissolved in a solvent; the obtained solutions are mixed and the reaction is stirred at a constant temperature; after the reaction is completed, an anti-solvent is added for crystallization, suction filtration is performed, and the precipitate is collected, washed and dried to obtain a 4,4'-bipyridyl ester salt compound. Wherein, compound 1 and compound 2 respectively include one or more of methyl 2-chloroacetate, methyl 2-bromoacetate, ethyl 2-chloroacetate and ethyl 2-bromoacetate. The 4,4'-bipyridyl ester salt compound provided by the present invention has high-efficiency herbicidal performance under neutral conditions and can be used as an active substance for controlling weeds in the soil environment; in an acidic environment, it can be rapidly degraded to avoid harm to the human body. It has significant advantages such as a simple synthesis method, low production cost, high yield, and no harmful residual substances left after use, and can be used as a safe and friendly new herbicide.

The application provides preparation and application of a polyphosphazene-based hydrogel with inherent antibacterial property, which is prepared by modifying polyphosphazene with ethyl bromoacetate to obtain a quaternary ammonium salt grafted polymer PZBA, and is formed by crosslinking of the quaternary ammonium salt grafted polyphosphazene-based polymer (PZBA) and polyvinyl alcohol (PVA). The polyphosphazene-based hydrogel (PZBA-PVA hydrogel) of the application can down-regulate pro-inflammatory cytokines, has an anti-inflammatory effect, and up-regulates the expression level of growth factors to promote tissue regeneration. The hydrogel prepared by the application has good tissue adhesion, biocompatibility and antibacterial property, plays an antibacterial and wound healing promoting role on infected wounds, and can be used for preparing antibacterial and wound healing promoting drugs.

The invention relates to a preparation method of DOTA-PNP, and belongs to the technical field of material synthesis. Cheap cycleanine is used as a starting raw material and reacts with tert-butyl bromoacetate to generate a tri-substituted product, the tri-substituted product is further substituted with ethyl bromoacetate to obtain a tetra-substituted product, ethyl ester is further hydrolyzed to obtain substituted carboxylic acid, the substituted carboxylic acid and p-nitrophenol are condensed, and finally tert-butyl is removed to obtain a target product.

The invention relates to the field of chemical synthesis, and particularly discloses a synthesis method of 6-(difluoromethyl)-2hydrogen-1, 2, 4-triazabenzene-3, 5-diketone and a preparation method of the 6-(difluoromethyl)-2hydrogen-1, 2, 4-triazabenzene-3, 5-diketone. The compound is shown as a formula I in the specification. Reacting the initial raw material a with liquid bromine to generate an intermediate b; protecting two amides on the intermediate b by using-PMB (p-methoxybenzyl) to obtain an intermediate c; reacting the intermediate c with ethyl bromodifluoroacetate to obtain an intermediate d; dissolving the intermediate d in DMSO, and decarboxylating at high temperature by using a fluid chemical technology to obtain an intermediate e; and removing PMB protection from the intermediate e, so as to obtain a final product 6-(difluoromethyl)-2hydrogen-1, 2, 4-triazine-3, 5-diketone, namely the 6-(difluoromethyl)-2hydrogen-1, 2, 4-triazine-3, 5-diketone. According to the method, the 6-nitrogen uracil which is low in price is used as a starting raw material, byproducts in each step in a synthesis route are extremely few, purification of each intermediate is relatively simple and convenient, and the total yield is increased to 44% from reported nine-step reaction 1.32% through linear five-step reaction, so that the method is a synthesis route with high atom economy.

The invention discloses an anionic fluorocarbon surfactant as well as a preparation method and application thereof, and belongs to the technical field of surfactants, the method specifically comprises the following steps: (1) in an argon atmosphere, dropwise adding hexafluoropropylene dimer and ethyl bromoacetate into a mixed solution of N-N dimethylacetamide, tetrabutylammonium bromide and potassium fluoride, and stirring to obtain a mixed solution; heating the reaction system at 80 DEG C for 24 hours, cooling to room temperature, and performing post-treatment to obtain a compound 1; (2) in an argon atmosphere, dissolving the compound 1 in absolute ether, dropwise adding into a Schlenk tube containing absolute ether and LiAlH4, stirring and reacting at room temperature for 3 hours, heating to 40 DEG C, stirring for 4 hours, cooling to room temperature, and post-processing to obtain a compound 2; and (3) dissolving the compound 2 and triethylamine in tetrahydrofuran, slowly dropwise adding chlorosulfonic acid, reacting for 3 hours in an ice-water bath, reacting for 6 hours at normal temperature, and performing post-treatment to obtain the sulfate anionic surfactant. The surfactant effectively solves the problems of environmental pollution and insufficient performance.