2067 results about "Alkylation" patented technology

The invention discloses a synthesis method of vitamin C ethyl ether, and belongs to the technical field of vitamin derivative synthesis. The synthesis method comprises the following steps: adding vitamin C, benzaldehyde and a catalyst into a first organic solvent, carrying out an aldolization reaction, adding an organic alkali after the aldolization reaction is finished, carrying out a neutralization reaction, adding an alkylation reagent, carrying out an alkylation reaction, and removing the first organic solvent after the alkylation reaction is finished, so as to obtain the vitamin C benzaldehyde. The preparation method comprises the following steps: adding a first organic solvent into a first organic solvent, pulping, filtering, collecting filter residues, washing and drying to obtain 5, 6-O-benzyl-3-O-ethyl-L-ascorbic acid, carrying out hydrogenation deprotection on the 5, 6-O-benzyl-3-O-ethyl-L-ascorbic acid, filtering after hydrogenation deprotection, collecting filtrate, crystallizing, collecting precipitate, washing and drying to obtain the 5, 6-O-benzyl-3-O-ethyl-L-ascorbic acid. The vitamin C ethyl ether is obtained. The synthesis method provided by the invention is simple to operate and high in production efficiency, and the obtained vitamin C ethyl ether is high in yield and purity.

The present invention uses commercially available 3-aminopropylsilane coupling agent, diallylamino polyether acrylate, and an alkylating agent, or γ-propanesultone, or γ-butyrolactone as raw materials, and through an aza-Michael addition reaction and a quaternization reaction, a multifunctional silane coupling agent containing one or more quaternary ammonium cations, or sulfobetaine, or carboxybetaine in its molecular structure is prepared, which is used for the surface modification of bioactive glass, and the bioactivity, antibacterial and antifungal properties, and hydrophilicity enhancement effects after the surface modification of bioactive glass are obtained.

The invention discloses a preparation method of a dual PDE3 / 4 inhibitor Encephaline. The preparation method comprises the following steps: carrying out a sizuki coupling reaction on initial raw materials of a compound shown as a formula 1 and a compound shown as a formula 2 to obtain a compound shown as a formula 3, carrying out intramolecular cyclization to obtain a compound shown as a formula 4, converting carbonyl into a compound shown as a formula 5 by using POCl3, and carrying out an alkylation reaction on the compound shown as a formula 5 and a compound shown as a formula 6 to obtain a compound shown as a formula 7. Wherein the acyl imine of the compound as shown in the formula 7 and a compound as shown in a formula 8 are subjected to substitution reaction to obtain the product Encephaline. The selected raw materials are easy to obtain, the operation method is simple and convenient, the product yield is high, and the method is suitable for batch production.

The embodiment of the invention provides a method for separating various phenols from cresol containing 2, 6-xylenol, which utilizes the characteristics that 2, 6-xylenol, 2, 4-xylenol, 2, 5-xylenol and isobutene can only generate mono-tert-butylated phenol, m-cresol, p-cresol and o-ethyl phenol, and o-cresol and isobutene can generate di-tert-butylphenol, and contains 2, 6-xylenol, 2, 4-xylenol, 2, 5-xylenol and 2, 4-xylenol. According to the method, cresol containing 2, 6-xylenol is subjected to the steps of monoalkylation, rectification, dialkylation, rectification, dealkylation, rectification and the like to realize separation of various phenols, so that the problem that the quality of m-cresol and p-cresol is influenced by 2, 6-xylenol when cresol extracted from medium-low temperature phenol-containing coal tar is separated is solved.

The invention discloses a modified amine curing agent and a preparation method thereof, and an epoxy resin composite material and a preparation method thereof, and belongs to the field of resin and composite materials. According to the curing agent, a C2-C8 alkyl chain is grafted to a methylene site of 4, 4 '-diaminodiphenylmethane (MDA) through free radical substitution and alkylation reaction, and a molecular structure with a flexible alkyl chain and a rigid benzene ring is formed. The preparation method comprises the following two steps: generating a halogenated intermediate from MDA and a halogen simple substance under certain reaction conditions, alkylating the halogenated intermediate with a Grignard reagent (RMgX), and purifying. The curing agent and epoxy resin are compounded, heated and cured, so that the epoxy resin composite material has relatively high impact strength and fracture toughness, has good tensile strength and hardness, has double functions of reinforcing and toughening, and solves the problem that reinforcing and toughening of traditional epoxy resin are difficult to be compatible; the method is suitable for the fields of aerospace, composite material adhesives and the like with harsh requirements on mechanical properties.

The invention discloses a magnetic ion exchange resin and a preparation method thereof, and the preparation method comprises the following steps: preparing a reaction solution which comprises magnetic particles, glycidyl methacrylate, divinylbenzene and a photoinitiator; the mass ratio of the glycidyl methacrylate to the divinyl benzene is (4.5-10): 1; an ultraviolet-initiated polymerization step: irradiating the reaction solution by ultraviolet light to initiate a polymerization reaction to obtain magnetic microspheres; a functional modification step: mixing the magnetic microspheres with an ammoniation reagent for ammoniation reaction to prepare ammoniated magnetic microspheres; and mixing the ammoniated magnetic microspheres with an alkylation reagent, and carrying out an alkylation reaction to prepare the magnetic ion exchange resin. According to the method, the production time is remarkably shortened, the extra energy consumption is reduced, and the process production flow is effectively simplified.

The invention relates to the technical field of antibacterial high polymer materials, in particular to an antibacterial nylon material as well as a preparation method and application thereof. The method comprises the following steps: carrying out anion ring-opening copolymerization on a seven-membered ring lysine monomer obtained by ring formation of lysine and a lactam monomer to obtain copolyamide, dissolving the copolyamide, and carrying out complete quaternization reaction by using halogenated hydrocarbon to obtain the antibacterial nylon material. The preparation method provided by the invention effectively avoids the problems of insufficient antibacterial property, obvious mechanical property reduction, poor thermal stability and the like of an antibacterial nylon material prepared by hydrochloric acid protonation in the prior art. Meanwhile, the seven-membered cyclic lysine monomer can be copolymerized without alkylation, the synthesis process is greatly simplified, the production efficiency is high, and the production cost is low. The prepared antibacterial nylon material has the characteristics of lasting and efficient antibacterial performance, high safety, environment friendliness, excellent mechanical property and thermal stability and the like, and can be widely applied to the fields of textiles, daily necessities, packaging materials, panels and the like.

An adhesive composition is shown and described herein. The composition comprises a silylated polyurethane, an epoxy functional compound, and an amine functional compound. The compositions are provided to control the molar ratio of amine active hydrogen (AH) to epoxy (E) groups. By controlling the amine active hydrogen to epoxy molar ratio, an adhesive with excellent adhesion and strength on a variety of types of substrates is provided.

This method for producing an aryl-alkylated indene composition involves: adding an arylalkyl group having a polymerizable unsaturated bond-containing group to an indene compound; and adding an arylalkyl group having no polymerizable unsaturated bond-containing group to the indene compound to which the arylalkyl group having a polymerizable unsaturated bond-containing group is added.

The present invention provides a multifunctional silane coupling agent, which is prepared from commercially available 3-aminopropylsilane coupling agent, acryloxy polyetheramine, and one of an alkylating agent, polyether sulfonate, γ-propane sultone or γ-butyrolactone through Michael addition reaction and quaternization reaction. The multifunctional silane coupling agent is a new variety carrying zwitterions, quaternary ammonium cations and polyether chains, enriching the functions and application scope of silane coupling agents. It can endow some modified materials with surface hydrophilicity, conductivity, antibacterial, antifogging, antifouling, biocompatibility, anticoagulant and wet lubrication properties, etc. at the same time.

The invention discloses a method for preparing tert-butyl ethylbenzene through alkylation of ethylbenzene and isobutene. In a reactor, a raw material containing ethylbenzene and isobutene is in contact with a catalyst for an alkylation reaction to obtain a product containing tert-butyl ethylbenzene, by changing the proportion of the shell ZSM-12 molecular sieve in the hydrogen-type Beta-coated ZSM-12 core-shell molecular sieve and combining high-temperature water vapor treatment, the obtained catalyst shows excellent catalytic performance in liquid-phase alkylation reaction of ethylbenzene and isobutene. The catalyst preparation process is simple to operate and easy for industrial production. The development of a p-tert-butyl ethylbenzene production technology is favorably promoted.

The invention discloses a method for efficiently preparing an ionic super-crosslinked polymer by a mechanochemical method as well as a product and application of the ionic super-crosslinked polymer, and belongs to the technical field of polymer material preparation. The preparation method comprises the following steps: adding a nitrogen-containing monomer, a cross-linking agent and a catalyst into a good solvent to obtain a reaction solution; carrying out planetary ball milling treatment on the reaction liquid, and carrying out a Friedel-Crafts alkylation reaction; and after the reaction is completed, recovering and purifying the product to obtain the ionic super-crosslinked polymer. The ionic super-crosslinked polymer prepared by the preparation method disclosed by the invention has a highly crosslinked and abundant pore structure, and meanwhile, the ionic super-crosslinked polymer has the performance advantages of good adsorption performance, excellent chemical stability and high thermal stability. The synthetic method of the ionic super-crosslinked polymer provided by the invention is efficient, energy-saving and environment-friendly, the product quality is high, and the method has wide popularization and application prospects.

The invention discloses a method for preparing aviation kerosene (aromatic hydrocarbon components) from biogas. The method comprises the following steps: separating biogas to obtain methane and carbon dioxide, and then carrying out a two-step chemical reaction process. The method comprises the following steps: firstly, carrying out dehydrogenation aromatization on methane to obtain aromatic hydrocarbon mainly containing benzene and hydrogen, and separating methane for circulating dehydrogenation aromatization reaction; then hydrogen and aromatic hydrocarbon are merged into carbon dioxide, and the polysubstituted aromatic hydrocarbon is obtained by coupling methanol synthesis and alkylation reaction of benzene without external source hydrogen. The method provided by the invention avoids the problem of low selectivity of aviation kerosene fraction hydrocarbons in a route of Fischer-Tropsch synthesis after methane and carbon dioxide are converted into synthesis gas. According to the conversion method for highly coupling the reaction processes, a new route for producing sustainable aviation kerosene from biogas is developed.

The invention belongs to the technical field of nuclear medicine molecular diagnosis and treatment, and discloses a modified CAIX targeting cyclic peptide, a nuclide marker and application of the modified CAIX targeting cyclic peptide in tumor diagnosis and treatment. According to the CAIX targeted cyclic peptide, a rigid bifunctional chelating agent RESCA is introduced to replace a traditional chelating agent, and a sulfonated or alkylated amino acid connector is combined, so that the enzymolysis resistance and in-vivo stability of the probe are remarkably improved. By optimizing the structure of the connector, the lipophilicity is reduced, liver and gall metabolism and non-specific uptake are reduced, and the high uptake rate of tumor target tissues is maintained. The therapeutic nuclide marker of the cyclopeptide can be used for intratumoral irradiation therapy using DOTA or NOTA in combination with an alkylated amino acid linker or an albumin ligand. Experiments show that the marker has high radiochemical purity, excellent pharmacokinetic characteristics and low kidney retention, and is suitable for precise diagnosis and targeted therapy of CAIX high expression tumors such as kidney cancer, colorectal cancer and brain glioma.

The invention relates to a method for preparing cyclohexanone by conversion of acetone and 1, 3-propylene glycol, and belongs to the technical field of chemical engineering. The method comprises the following steps: catalyzing a dialkylation reaction of acetone and 1, 3-propylene glycol by virtue of a supported nickel or palladium catalyst and a potassium phosphate cocatalyst, and removing water from acetone and 1, 3-propylene glycol which are equal in molar weight, so as to obtain cyclohexanone. The method contributes to the production of bulk chemicals and fine chemicals by a fermentation method, and makes a contribution to the strategic goal of low-carbon development.

The invention provides a synthetic method of high-purity p-methylstyrene. The method comprises the following steps: carrying out alkylation on toluene and catalytic dry gas in a modified ZSM-5 catalyst to generate methyl-ethylbenzene, carrying out adsorption separation on the methyl-ethylbenzene to obtain high-purity p-methyl-ethylbenzene, and carrying out high-temperature dehydrogenation on the p-methyl-ethylbenzene in the presence of an iron-based catalyst to obtain the high-purity p-methyl styrene. According to the method, based on the synergistic effect of a preparation process and an alkylation reaction catalyst, the para-selectivity of the alkylation reaction catalyst is strictly controlled, so that the selectivity of the catalyst is ensured, the service life of the catalyst is greatly prolonged, and furthermore, a simulated moving bed is utilized to adsorb and separate methyl ethylbenzene isomers, separate, purify and recycle; the raw material utilization rate and the product purity are improved, and the purity of the finally obtained p-methylstyrene is 99% or above.

The invention provides a chemically modified tetanus toxin C fragment as well as preparation and application thereof. The method for chemically modifying the tetanus toxin C fragment comprises the following steps: 1) reacting the tetanus toxin C fragment with a reducing agent to reduce a disulfide bond in the tetanus toxin C fragment; and 2) carrying out a reaction on the reduced tetanus toxin C fragment and an alkylation reagent, and carrying out modification. The recombinant tetanus toxin C fragment prepared by the method disclosed by the invention not only meets the quality standard required by pharmacopeia, but also has the advantages of stable conformation, high yield, easiness in amplification and low cost, and has a wide application prospect in the preparation of human vaccines, veterinary vaccines and antibody drugs and the development process of in-vitro diagnostic reagents.

The invention discloses an LC-MS / MS detection method for a palbozuril monoclonal antibody drug in a blood sample, which comprises the following steps: enriching and purifying the palbozuril monoclonal antibody drug in serum and plasma by coupling an enrichment reagent I with magnetic beads, magnetically separating the enriched blood sample, discarding the supernatant, adding a buffer solution I for leaching, and adding a buffer solution II for diluting after leaching; the method comprises the following steps: carrying out high-temperature denaturation on a diluted blood sample, sequentially adding an internal standard and protease for enzymolysis, and then adopting a high performance liquid chromatography-tandem mass spectrometry to realize high-sensitivity rapid detection of the drug concentration of the palbozuril monoclonal antibody in the blood sample. In the pretreatment process, the steps of protein reduction and alkylation are removed, the proteolysis time is shortened, the whole process is simple, convenient and rapid, and multiple requirements of clinical detection on timeliness, accuracy and low detection cost can be met at the same time.

The invention belongs to the technical field of heat-conducting fillers, and particularly relates to a modified hexagonal boron nitride compound as well as a preparation method and application thereof. The modified hexagonal boron nitride compound provided by the invention comprises alkylated aluminum oxide microspheres and hydroxylated hexagonal boron nitride nanosheets coated on the surfaces of the alkylated aluminum oxide microspheres. The alkylated aluminum oxide microspheres are combined with the hydroxylated hexagonal boron nitride nanosheets through an adsorption effect, so that the hydroxylated hexagonal boron nitride nanosheets coat the surfaces of the alkylated aluminum oxide microspheres in a lap joint manner, and the dispersity of the modified hexagonal boron nitride is improved. The hydroxylated hexagonal boron nitride nanosheets which are mutually lapped can construct a phonon transmission channel, so that smooth transmission of phonons is facilitated, and the heat conductivity coefficient of the material is improved; meanwhile, on the basis that the original structure of the alkylated alumina microspheres is kept unchanged, dense accumulation among particles can be promoted, and a well-connected heat conduction network is formed, so that the interface thermal resistance is reduced, and the heat conductivity coefficient of the material is further improved.

The invention discloses a synthesis process of vitamin C ethyl ether, and belongs to the technical field of vitamin C derivative synthesis. The process comprises the following steps: taking L-ascorbic acid as a raw material, adding acetone, anhydrous cupric sulfate and acetyl chloride, and reacting for 1-2 hours at 38-40 DEG C under the protection of nitrogen to obtain a vitamin C protector; adding alkali, water, an alkylating reagent and absolute ethyl alcohol into the reaction product, reacting for 3 hours at 75-78 DEG C under the protection of nitrogen, and performing reduced pressure distillation to obtain a vitamin C protector etherate; and finally, hydrolyzing by using cationic resin, removing a protecting group, and recrystallizing by using ethyl acetate to obtain the vitamin C ethyl ether. Through the synergistic catalysis of anhydrous cupric sulfate and acetyl chloride, the reaction time is remarkably shortened, and the product purity and yield are improved. Through detection, the product purity is more than 99.5%, the total yield can reach more than 80%, and an efficient and economical method is provided for industrial production of vitamin C ethyl ether.

The invention discloses synthesis and antitumor activity research of a novel drug small molecular formula (1) containing a phenothiazine structure. R is # imgabs 1 #. 10H phenothiazine is used as an initial raw material, (E)-3-(10-ethyl-10H-phenothiazin-3-yl) acrylic acid is generated through a typical Friedel-Crafts alkylation reaction, an NBS bromination reaction and the like, and then an important intermediate compound 6 is synthesized through a Wittig reaction and a hydrolysis reaction. And carrying out coupling reaction on the intermediate compound 7 and different amine compounds to obtain 11 target compounds 7a-7k: formula (1). A CCK-8 experiment is carried out on a target compound to obtain a conclusion that the target compound 7a-7k and 5-fluorouracil are tested at the concentration of 20 mu M, and the result shows that the compound 7f has the best inhibition effect on A549, Hep G2 and HeLa cells, and the compound 7c has the better inhibition effect on the A549 cells. IC50 value calculation is carried out on a target compound under various concentrations, the IC50 value of 7c to HELA cells is small, the IC50 value of 7f to Hep G2 and HeLa cells is minimum, and the inhibition effect is the best. Therefore, the compound can be used for antitumor drugs.

The present invention relates to the field of optical imaging. More specifically, the present invention relates to a class of monoalkylated cyanine dyes having red to near-infrared (650-900 nm) emission, characterized by pH responsiveness, and to conjugates thereof with biological ligands. The present invention also relates to the use of these compounds as optical diagnostic agents in the imaging or therapy of solid tumors, to methods for their preparation and to compositions containing them. The monoalkylated cyanine dyes have the general formula (I), in which R1 and R3 are independently selected from the group consisting of hydrogen, -SO3H, -COOH and -CONH-Y; and R2 and R4 are hydrogen, or R1 together with R2 and R3 together with R4 both form two aryl rings optionally substituted by 1 to 4 -SO3H groups together with the atoms to which they are bonded; R5 is an alkyl group optionally substituted by a group selected from -SO3H, -COOH and -CONH2. #imgabs0#

This resist composition contains: a resin component (A1), the solubility of which in a developer solution changes due to the action of an acid; and a compound (D0) represented by general formula (d0-1). In the formula, Ar is an aromatic ring; OH is a hydroxy group; Xd01 is an iodine atom, a fluorine atom, a bromine atom, or a fluorinated alkyl group; Ld is a single bond or a divalent linking group; Z+ is S+ or I+; and Xd02 is an iodine atom, a fluorine atom, a bromine atom, or a fluorinated alkyl group. [Chemical formula 1]

The invention discloses polyether modified silicone oil for improving polyol compatibility and application of the polyether modified silicone oil in a polyurethane foam composition. The structure of the polyether modified silicone oil simultaneously comprises the following chain segments: (a) a polyoxyethylene ether chain segment; and (b) alkylated polyoxyethylene polyoxypropylene ether chain segments, wherein EO and PO can be random copolymerization or block copolymerization. Wherein the molar ratio of the polyoxyethylene ether chain segment to the alkylated polyoxyethylene polyoxypropylene ether chain segment is 1: (0.6-4), preferably 1: (1-2). The polyurethane composition comprises a component A and a component B, the component A is an isocyanate reactive component and comprises polyol, a catalyst, a foaming agent and polyether modified silicone oil; and the component B is an isocyanate component. The polyether modified silicone oil has the functions of a compatilizer and a foam stabilizer, and a polyurethane composition has good storage performance and foaming stability and can be used for preparing a polyurethane foaming material.

The invention provides an efficient preparation method of hydrophobic chitosan. Chitosan can be directly alkylated to realize efficient synthesis of the hydrophobic chitosan only through one-step reaction. Compared with an existing indirect synthesis mode, the method has the advantages that firstly, extra consumption generated by any intermediate step is not needed, namely, the hydrophobic chitosan is efficiently synthesized by a one-pot one-step method; secondly, not only is amino in the chitosan directly alkylated, but also hydroxyl which cannot be indirectly alkylated can be alkylated to generate hydrophobic chitosan with both N-alkylated and O-alkylated, and the hydrophobic chitosan obtained by the method has more efficient hemostatic performance. Therefore, the method for producing hydrophobic chitosan through direct alkylation is more efficient, higher in yield, low in cost and more excellent in performance.

The invention relates to the field of feeding, and discloses a feeding system and a feeding method for intermediate synthesis, and the feeding method comprises the following steps: based on monitoring and analyzing the distribution condition of a catalyst bed layer in an alkylation process, establishing an inactivation model in combination with pressure fluctuation to dynamically compensate the activity of a catalyst, and adjusting the dispersity and the feeding speed of the catalyst through the inactivation model; based on the end of alkylation, obtaining the oxidant concentration in the oxidation process, establishing a target function with the reaction time based on the oxidant change rate, calculating the reaction time deviation degree through the target function, and intelligently adjusting the oxidant supply frequency in combination with analysis; feeding parameters of a plurality of historical reaction periods are obtained, deep collaborative optimization is carried out on the reaction time and the feeding parameters by establishing a three-layer intelligent regulation and control model, and a time scale correlation inactivation model and a time scale coupling free radical prediction model are constructed to solve the optimal adjustment amount; and carrying out real-time self-adaptive regulation and control on feeding parameters, and integrating prediction maintenance to carry out feedback iteration.

The invention discloses a method for resource utilization of fluorine-containing waste gas in hexafluoropropylene oxide production and co-production of hydrofluoroether, which comprises the following steps of: firstly, reacting the fluorine-containing waste gas in hexafluoropropylene oxide production under the action of a fluorine ion catalytic system to generate a perfluorinated intermediate product; then, the perfluorinated intermediate product reacts with an alkylating reagent under the action of a fluorinating reagent to produce a hydrofluoroether product. Hydrofluoroether products with different structures are obtained by utilizing the characteristics of nucleophilic addition reaction of a by-product acyl fluoride and hexafluoropropylene in the production of hexafluoropropylene oxide and utilizing the characteristics of the addition product for preparing hydrofluoroether by using the same alkylation process; the hydrofluoroether products are widely applied to the fields of semiconductor temperature control fluid, data center immersion heat exchange fluid, electrified cleaning agents and inert diluents of base stations or weak current equipment and the like, and have high added value.

The invention belongs to the technical field of compound synthesis, and particularly relates to a synthesis method of AEA-AEA. Triethylene glycol is adopted as a starting material, in the first step, p-toluenesulfonate with high leaving property is formed through TsCl, then nucleophilic substitution is performed, and a product 2 is obtained; the preparation method comprises the following steps: preparing a product 3, oxidizing by adopting TEMPO capable of being industrially produced, removing Pht through quantitative hydrazine hydrate to obtain a product 4, esterifying and extracting to obtain a product 5, acylating through the product 3 to obtain amide, washing, extracting and pulping to obtain an esterified product 6; and finally, quantitatively removing Pht, hydrolyzing and pulping to obtain a pure product. According to the method, complex operation steps of using metal hydride and alkylating column passing are avoided, process production can be realized, and the product yield and purity are relatively high.

The invention belongs to the field of chemical production, and particularly relates to a method for catalytically synthesizing propiconazole by using ionic liquid. And carrying out condensation reaction on the brominated substance 2-bromomethyl-2-(2, 4-dichlorophenyl)-4-propyl-1, 3-dioxopentane and triazole under the catalysis of the ionic liquid to generate propiconazole. The ionic liquid is one of [Emim] BF4, [Emim] PF6, [BMIM] PF6 and [BMIM] OH. According to the invention, the imidazole cation ionic liquid is used as a catalyst and a solvent to catalyze the N-alkylation reaction of 2-bromomethyl-2-(2, 4-dichlorophenyl)-4-propyl-1, 3-dioxopentane and triazole, and the research finds that the alkaline imidazole cation liquid has good catalytic performance, high yield and good selectivity, and can be used as a catalyst for catalyzing the N-alkylation reaction of 2-bromomethyl-2-(2, 4-dichlorophenyl)-4-propyl-1, 3-dioxopentane and triazole. And the reaction conditions are mild, the operation is simple, the ionic liquid is easy to recover, and the catalytic activity is not obviously reduced after being applied for five times.