1224 results about "Sulfonyl chloride" patented technology

The invention relates to a method for preparing a polymer separating film, and in particular relates to a method for preparing an acid-proof polysulfonamide nanofiltration composite film, wherein a polysulfonamide ultra-thin functional separating layer is condensed and compounded through an interface between heterocyclic polyamine and poly-naphthalene sulfonyl chloride on a porous support film according to certain processing steps by controlling certain technological conditions. The method has the following advantages: the selective separating performance and the penetrating quality of the nanofiltration composite film are not lower than those of the existing polysulfonamide nanofiltration composite film; moreover, the acid resistance is superior; and simultaneously, the preparation method is relatively simple. The acid-proof polysulfonamide nanofiltration composite film can be widely applied to the separation of various types of liquids, specifically the separation of acid industrial fluids; and the method is wide in application.

The invention discloses an oxidized graphene material modified by a water-soluble anthraquinone compound and a preparation method of the graphene material and belongs to the technical field of water treatment of environmental engineering. The mass percent of the water-soluble anthraquinone compound in the material is 1-5%. The preparation method comprises the following steps: dispersing oxidized graphene into de-ionized water; adjusting the pH (Potential of Hydrogen) to 9-11 by using ammonia water; adding diethylenetriamine and reacting under a water bath condition at the temperature of higher than 95 DEG C; drying to obtain amino-modified graphene powder; dispersing the amino-modified graphene powder into a mixed solution of dichloromethane and absolute ethyl alcohol with the volume ratio of not more than 1 to obtain a mixed system in which the mass volume percent of the amino-modified graphene is 0.1%; and adding a dichloromethane solution of an anthraquinone compound containing a sulfonyl chloride radical and reacting at a room temperature. The material has a very good catalytic performance and the anaerobic organism conversion speed of organic matters which are difficult to degrade can be improved; the secondary pollution problem to the environment, caused by the loss of the water-soluble anthraquinone compound, is solved.

The invention discloses a polysulfonamide nanofiltration or reverse-osmosis composite membrane, and a preparation method thereof. the preparation method for the polysulfonamide nanofiltration or reverse-osmosis composite membrane comprises the following steps: pretreatment of a porous supporting membrane; alternate layer-upon-layer assembling of a sulfonyl chloride organic-phase solution and a polyamine water-phase solution on the surface of the porous supporting membrane via reaction; heat treatment; etc.; wherein heat treatment can be carried out during or after layer-upon-layer assembling. Nanoparticles, a surfactant, a catalytic acid absorbent or catalyst, a pore forming agent and other additives are added into the sulfonyl chloride organic-phase solution and the polyamine water-phase solution. The polysulfonamide nanofiltration or reverse-osmosis composite membrane prepared by using the method has improved desalination performance and acid resistance, smoother surface and lower roughness compared with composite membranes prepared through traditional interfacial polymerization, and has good application prospects in the fields of nanofiltration and reverse osmosis.

The invention relates to a method for synthesizing and purifying Fasudil hydrochloride, comprising the following steps of: adding N,N-dimethylformamide and thionyl dichloride to 5-isoquinoline sulfonic acid to obtain a 5-isoquinoline sulfonyl chloride hydrochloride; adding the 5-isoquinoline sulfonyl chloride hydrochloride, water and sodium bicarbonate to dichloroethene to obtain a 5-isoquinoline sulfonyl chloride solution; dripping the 5-isoquinoline sulfonyl chloride solution to homopiperazine at zero DEG C to obtain a hexahydro-1-(5-sulfonyl isoquinoline)-1(H)-1,4-benzodiazepine solution; removing impurities in three steps; adjusting the pH value to be 4.5-5.5 with an acidizing fluid, extracting, and discarding an organic phase dissolved with a dipolymer impurity; adjusting the pH value to be 9.5-10.5 with alkali, extracting and discarding a water phase dissolved with homopiperazine impurities and a majority of pigments; removing the residue pigment by passing through silica gel; and finally, washing, drying, filtering, then dripping a hydrochloric acid-ethanol solution at 0 DEG C, and crystallizing while stirring to prepare the Fasudil hydrochloride. The invention has the advantages that the three kinds of impurities are effectively removed through the three-step purification process, and the purity of a product reaches more than 99.9%.

The invention discloses a synthetic process of 1-chloro-cyclopropanecarbonyl chloride, which belongs to the technical field of fine chemical processes. The process is implemented by taking alpha-acetyl-gamma-butyrolactone and sulfonyl chloride as raw materials through the steps of chlorinating, ring cleavage, cyclization, and re-chlorinating, so that a target product is obtained. The synthetic process is implemented by taking cheap industrial chemicals as raw materials and reaction reagents, and by using a single solvent system, a smooth process connection is achieved, so that the reaction yield is improved, the process operation is simplified, the cost of raw materials is reduced, and the cost of production is lowered.

The N-arylsulfilimine-catalyzed coupling of aromatic sulfonyl chlorides with N-([1,2,4]triazolopyrimidin-2-yl)amines to form N-([1,2,4]triazolo-pyrimidin-2-yl)aryl sulfonamides is improved by the selection of 3-picoline or 3,5-lutidine as the base.

The invention relates to a vinylene carbonate preparation method, which comprises the following steps: synthesizing monochloroethylene carbonate (C1EC), adding sulfonyl chloride drop by drop on ethylene carbonate (EC) under existence of an initiator azo, wherein mol ratio of sulfonyl chloride to EC is 1.1-1.2: 1, adding temperature is 55-80 DEG C, adding time is 5-6 hours, insulating for 1 hour, adding trialkylamine for 6-7 hours in a solution of dimethyl carbonate (DMC) and ClEC crude product according to weight ratio of 2.5-2.5: 1, wherein the addition temperature is 50-59 DEG C, insulating for 10-12 hours, wherein weight ratio of trialkylamine to ClEC is 1:1-1.1, and performing vacuum rectification and toluene recrystallization for purifiying VC. According to the invention, EC conversion rate can reach more than 94%, VC yield can reach 44%, and purity can reach more than 99.9%. The method has the advantages of simple process flow, mild technology condition, low reaction temperature and increased production security. In the invention, DMC is especially employed as solvent product which is easy to be separated.

The invention discloses a preparation method of a porous inorganic filling materials-fixed quinone compound, belonging to the technical field of water treatment in environmental engineering. The method comprises the following steps of: selecting porous inorganic filling materials such as ceramsites, volcanics and the like; plating gamma-aluminum oxide on the surface of the materials; aminating, so that the surfaces of the porous inorganic filling materials contain a certain quantity of primary amidogen; putting the aminated materials into hydrochloric solution to have reaction for protecting the primary amidogen; and putting the reacted porous inorganic filling materials into sodium hydroxide solution, adding sulfonyl chloride group-containing anthraquinone compound which is dissolved in dichloromethane, and reacting for 6-10h under the room temperature to fix the water-soluble quinone compound. The quinone compound-containing macroporous polymer is applied to an anaerobic reactor to be capable of improving the biotransformation speed of an organic matter which is hardly degraded. The method covalently fixes the quinone compound on the macroporous polymer of a biologic carrier, so that the redox medium is easily contacted with the microbe, thereby overcoming the problem of the secondary pollution since the water-soluble quinone compound flows out with the water.

The invention relates to a method for preparing ethylene sulfate. The method comprises the following steps: S1, carrying out a nucleophilic substitution reaction: carrying out the nucleophilic substitution reaction on ethylene glycol and sulfonyl chloride, which are used as starting raw materials, with trichloromethane as solvent to obtain crude ethylene sulfate; and S2, refining and purifying: dissolving the crude ethylene sulfate in trichloromethane, heating and refluxing the obtained solution under the protection of nitrogen to completely dissolve the crude ethylene sulfate, performing cooling recrystallization, performing filtration, and carrying out reduced pressure drying on the obtained filter cake to obtain the crude ethylene sulfate. Compared with the prior art, the method for preparing the ethylene sulfate from the ethylene glycol and sulfonyl chloride through a one-step reaction without a catalyst has the advantages of short reaction route, mild reaction conditions, simple synthesis process, easiness in operation, high safety, simple and easily-available raw materials, low cost and few byproducts; and the prepared product has the advantages of high purity, low moisture content, low acid value, and suitableness for being industrially produced.

The invention relates to a fasudil hydrochloride compound and a novel method thereof. The method comprises the following steps of: in the presence of a solvent, performing sulfonation reaction on a chlorosulfonic acid serving as a sulfonating agent and isoquinoline to generate a 5-isoquinolinesulfonic acid; reacting the 5-isoquinolinesulfonic acid with thionyl chloride under a heating condition to generate isoquinoline-5-sulfonyl chloride hydrochloride; and dissolving the isoquinoline-5-sulfonyl chloride hydrochloride with ice water, adjusting the pH value of the solution with sodium bicarbonate, reacting the solution with homopiperazine, adjusting the pH value again with a hydrochloric acid, and concentrating under reduced pressure and recrystallizing to prepare the fasudil hydrochloride compound. The synthesis method of the invention has the advantages of mild reaction conditions, high yield and easy industrial production.

The present invention provides a production method of benzenesulfonyl chloride. It is characterized by that said invention uses benzene and chlorosulfonic acid as raw material, and makes them undergo the processes of sulfonation reaction, hydrolytic dilution, standing still and layer separation and reduced pressure distillation so as to obtain the invented product. Said invention also provides the concrete steps of every process and its concrete requirements.

The invention discloses a method for synthesizing Imatinib. In the method, 4-methylol-N-[4-methyl-3-aminophenyl] benzamide is used as the raw material to carry out addition reaction with cyanamide to obtain an intermediate 4-methylol-N-(3-guanidyl-4-methylphenyl) benzamide (II), the intermediate (II) carries out condensation reaction with 3-(3-dimethylamino allyl acyl) pyridine to obtain an intermediate 4-methylol-N-[4-methyl-3-[[4-(3-pyridine)-2-pyrimidine] amino] phenyl] benzamide (III), the intermediate (III) reacts with substituted benzene sulfonyl chloride to obtain an intermediate 4-[ substituted benzenesulfonic acid carbomethoxy]-N-[4-methyl-3-[[4-(3-pyridine)-2-pyrimidine] amino] phenyl] benzamide (IV), and finally the intermediate (IV) reacts with methylpiperazine to obtain the Imatinib (V). The method has simple route process, mild conditions, high product purity and yield, and comparatively low cost and is beneficial to industrialized production.

The invention discloses a synthesis and preparation method of fasudil hydrochloride, which comprises the steps of taking 5-isoquinoline sulfoacid as raw material, refluxing in thionyl chloride to obtain 5-isoquinoline sulfonyl chloride hydrochloride, adding dichloromethane after dissolving with ice water, adjusting pH value of the solution to be neutral and performing liquid eparation; washing organic phase with water and edible salt, drying and filtering to obtain dichloromethane solution of 5-isoquinoline sulfonyl chloride; performing reaction of the solution with high purity piperazine in the presence of other alkaline reagents, washing the reaction solution with hydrochloric acid aqueous solution and sodium hydroxide aqueous solution after reaction, and extracting the washing solution respectively with dichloromethane; combining organic phases, washing with water, drying and filtering, and dropwise adding saturated hydrogen chloride ethanol solution to separate out crude product of fasudil hydrochloride; and recrystalizing the crude product with ethanol aqueous solution to obtain fasudil hydrochloride. The method provided by the invention greatly reduces the usage amount of high purity piperazine that is expensive by using deacidifying agents that are low in cost so as to reduce the preparation cost of fasudil hydrochloride effectively.

The invention discloses a water-solubility macromolecular chelant containing sulfourea group and a preparation method thereof. The chelant of the invention is prepared by the following method: (a) adjusting the pH value of formaldehyde with acid liquor to activate the formaldehyde; (b) adding the sulfourea, adjusting the pH value with alkali, and reacting at the temperature of 75-90 DEG C; (c) adjusting the pH value with the acid, adding the alcoholic solution of benzene sulfonyl chloride to react at 70-90 DEG C; (d) reducing temperature to 50-60 DEG C, adjusting the pH value with the alkali, and reducing the temperature to below 40 DEG C to prepare the chelant. The chelant of the invention has chelation sedimentation function to almost all of the transition stated heavy metals, which can not only be used in the treatment of the heavy metal sewage containing copper, zinc, nickel, mercury, cadmium, and the like, but also can be used in the stabilization treatment of the heavy metal in the solid wastes such as mud, waste incineration flying ashes, and the like. The preparation method of the invention has the advantages of no need of high temperature and high voltage, low one-time investment, easy availability of raw materials, and zero waste gas, waste liquid and waste residue in the production process.

The invention provides an ultraviolet positive photoresist suitable for exposure under a UV light source. The photoresist is composed of, by mass percent, 1 to 10% of diazonaphthoquinone sulfonate photosensitizer with special structure, 10 to 50% of linear phenolic resin, 0.2 to 1% of sensitizer, 0.1 to 1% of toughening agent, 0.4 to 1% of adhesion promoter, 0.2 to 1% of leveling agent and the balance of solvent; wherein the diazonaphthoquinone sulfonate photosensitizer with special structure is obtained by subjecting 1, 1- P-hydroxyphenyl-[1-Biphenyl group-4-Isopropyl group-(1-o-methyl-4-phenol)] propane and 2-Diazo-1-Naphthoquinone-5-sulfonyl chloride to substitution reaction or esterification reaction according to the ratio of 1: 2; The linear phenol-formaldehyde resin is a mixture oflinear phenol-formaldehyde resin 1 and linear phenol-formaldehyde resin 2, and the weight ratio of linear phenol-formaldehyde resin 1 and linear phenol-formaldehyde resin 2 is 2-8: 8-2. The ultraviolet positive photoresist of the present invention has higher resolution, photosensitivity and size reducibility than the conventional diazonaphthoquinone sulfonate Phenolic resin system photoresist.

The invention relates to a organosilicon waterproof emulsion for construction and a preparation method thereof, and is characterized in that 1 portion to 100 portions of siloxane which contains active group is modified by adding 1 portions to 40 portions of sulfonyl chloride with hydrophobic group under 0.1 portions to 10 portions of catalyst. The modified siloxane and 4 portions to 100 portions of silane coupling agent and emulsifier are emulsified in water to make a construction waterproof material of micro-emulsion water base with an average diameter less than 1nm and 10 percent to 80 percent of effective components; the construction waterproof material can dilute with water at any ratio and has two years stable period for room temperature storage. The organosilicon waterproof emulsion of the invention is applicable to mineral basement such as bricks, stones, concretes, and mortar which are all required to be shielded against water. The spraying or brushing can be used in the invention for waterproofing application of external and internal walls of buildings, roofs, floors, basements, etc. The emulsion of the invention has the advantages of low cost, no pollution, long service life, good waterproof performance without changing matrix color, being able to reduce water absorption and decrease spalling caused by freeze-thaw and weathering and prolonging basement service time. The invention has low cost, is environment-friendly and has remarkable social and economic benefit.

The invention provides an aromatic polymer sulfonamide. The above polymer adopts an aromatic polymer as a main chain, and the side chain of the polymer contains a sulfonamide group. The sulfonamide group is hydrophobic, can dissociate at a high temperature to provide protons, and cross-links with an acyl chloride group, a sulfonyl chloride group and a phosphoryl chloride group, so the aromatic polymer sulfonamide has the advantages of good barrier, good conductivity and good mechanical strength as a film material, and has good application prospects in fields of fuel batteries, flow batteries, electrodialysis and solid acid catalysts.

The invention discloses a preparation method of S-aryl phosphorothioate. The preparation method comprises the following steps of (1) adding a copper catalyst, an aryl sulfonyl chloride and phosphite in an organic solvent, reacting for 12-24 h at a temperature of 60-150 DEG C and cooling to a room temperature to obtain a reaction liquid; and (2) concentrating the reaction liquid, separating and purifying to obtain S-aryl phosphorothioate. According to the preparation method of S-aryl phosphorothioate, a one-pot method is adopted; copper is used as the catalyst; economical and easily available aryl sulfonyl chloride and phosphite are used as the raw materials; and a coupling reaction is carried out directly to generate corresponding S-aryl phosphorothioate, without adding alkali in air. A synthetic system has a relatively wide application scope, is compatible with a plurality of groups such as alkoxy, aryl, halogen and acyloxy. The preparation method provided by the invention is simple in process, convenient for operations and mild in reaction conditions, has a wide substrate range and relatively high yield, and is suitable for popularization and application.

The invention discloses a preparation method of fasudil hydrochloride. The preparation method comprises the following steps of: performing sulfonylation on 5-isoquinoline sulfonyl chloride and amino-protected homopiperazine, and removing an amino protective group of a reaction product. The amino-protected homopiperazine is taken as a raw material for the sulfonylation, so that two amino groups are prevented from being subjected to the sulfonylation to generate a byproduct; therefore, the yield of a target product (namely the fasudil hydrochloride) is improved, and the obtained product has high purity.

The invention provides a preparation method of trifluoro methanesulfonic anhydride. The method comprises the following steps of: firstly reacting trifluoro methanesulphonyl fluoride with alkali metal hydroxide to prepare trifluoro mesylate, purifying trifluoro mesylate by recrystallization by utilizing an organic solvent, reacting trifluoro methane sulfonyl chloride with trifluoro mesylate to generate a trifluoro methanesulfonic anhydride crude product, and finally purifying trifluoro methanesulfonic anhydride by atmospheric distillation. The preparation method of trifluoro methanesulfonic anhydride can be used for not only effectively simplifying reaction steps so that the operation process is simple and convenient and the operation is safe, but also avoiding byproducts generated in the process of the traditional method for producing trifluoro methanesulfonic anhydride, and effectively reducing the contents of F<-> and SO4<2-> in the product; by utilizing recrystallization, atmospheric distillation and other methods for purification, the product purity is up to 99.5%; and more importantly, the yield of anhydride is greatly increased and raised to 88% from original 60%.

The invention belongs to the technical field of medicine, and relates to a guanidinylation SS-PAAs gene vector polymer as well as preparation and application thereof. The preparation method comprises the following steps: the guanidinylation SS-PAAs gene vector polymer is finally prepared from a cross-linking agent with a dual-acroloyl structure and a guanidinylation reagent through the processes of protection reaction performed on sulfonyl chlorides by sulfonyl chlorides, Michael addition polymerization and removal of protection of a benzene sulfonyl chloride guanidyl protecting agent in sequence. The polymer gene vector can be self-assembled with different kinds of gene segments to form a compound, so that the excellent biological membrane permeability is achieved, and the responsive degradation is realized in the reducible environment of cells, and the nuclear localization effect is achieved. The capability of loading the gene segments of the vector and the transport process can be regulated through controlling the guanidinylation reagent species, the proportion of the guanidinylation reagent in the polymer, and the molecular mass. The guanidinylation SS-PAAs gene vector can improve the transfection efficiency of genes, and reduce cytotoxicity, and is a novel gene vector adopted in the process of gene therapy.

The invention relates to a synthetic method of deuterium-marked sulfanilamide. The method comprises the following steps of: reacting deuterated sulfonic acid with N-chlorosuccinimide (NCS) to obtain deuterated sulfonyl chloride which is not required to be separated; and adding amine for undergoing an amination reaction under the action of a metal catalyst to obtain deuterium-marked sulfanilamide. Compared with the prior art, the method has the advantages that: acyl chloride synthesis and the amination reaction are performed with a 'one pot process', operation is simple and convenient, the yield is high, and a synthesized product comprises sulfapyridine-benzene ring-D4, sulfadimidine-benzene ring-D4, sulfameter-benzene ring-D4, sulfaquinoxaline-benzene ring-D4, sulfisoxazole-benzene ring-D4 and sulfamethoxazole-benzene ring-D4.

The production process of p-acetamido benzene sulfonyl chloride as intermediate for sulfanilamide medicine includes the following steps: chlorosulfonating acetylaminobenzene as main material with chlorosulfonic acid to produce sulfonated oil and absorbing hydrogen chloride gas to prepare hydrochloric acid; separating sulfonated oil, adding water and decomposing chlorosulfonic acid to obtain separated oil while absorbing produced hydrogen chloride gas; separating the separated oil and adding water to deposit out p-acetamido benzene sulfonyl chloride; further separating, eliminating p-acetamido benzene sulfonyl chloride mother liquid, water washing the crystal while side producing sulfuric acid; using the side produced sulfuric acid in recovering p-amido benzene sulfonic acid; and reusing crystal eliminating water in the separation. The present invention realizes the comprehensive utilization, protects environment and lowers the cost.