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1229 results about "Sulfonyl chloride" patented technology

Sulfonyl halide groups occur when a sulfonyl functional group is singly bonded to a halogen atom. They have the general formula RSO 2 X where X is a halogen. The stability of sulfonyl halides decreases in the order fluorides > chlorides > bromides > iodides, all four types being well known. The sulfonyl chlorides are of dominant importance in ...

Industrial process for the synthesis of 17a-acetoxy-11ss-[4-(n,n-dimethyl-amino)- phenyl]-19-norpregna-4,9-diene-3,20-dione and new intermediates of the process

The present invention relates to a new industrial process for the synthesis of solvate- free 17a-acetoxy-11ss-[4-(N,N-dimethyl-amino)-phenyl]-19-norpregna-4,9-diene-3,20-dione [CDB -2914] of formula (I) which is a strong antiprogestogene and antiglucocorticoid agent. The invention also relates to compounds of formula (VII) and (VIII) used as intermediates in the process. The process according to the invention is the following: i) 3-(ethylene-dioxy)-estra-5(10),9(11)-diene-17-one of formula (X) is reacted with potassium acetilyde formed in situ in dry tetrahydrofuran by known method, ii) the obtained 3-(ethylene-dioxy)-17a-ethynyl-17ss-hydroxy-estra-5(10),9(11)-diene of formula (IX) is reacted with phenylsulfenyl chloride in dichloromethane in the presence of triethylamine and acetic acid, iii) the obtained isomeric mixture of 3-(ethylene-dioxy)-21-(phenyl-sulfinyl)-19-norpregna-5(10),9(11),17(20),20-tetraene of formula (VIII) is reacted first with sodium methoxide in methanol, then with trimethyl phosphite, iv) the obtained 3-(ethylene-dioxy)-17a-hydroxy-20-methoxy-19-norpregna-5(10),9(11),20-triene of formula (VII) is reacted with hydrogen chloride in methanol, then v) the obtained 3-(ethylene-dioxy)-17a-hydroxy-19-norpregna-5(10),9(11l); -diene-20- one of formula (VI) is reacted with ethylene glycol hi dichloromethane in the presence of trimethyl orthoformate and p-toluenesulfonic acid by known method, vi) the obtained 3,3,20,20-bis(ethylene-dioxy)-17a-hydroxy-19-norpregna- 5(10),9(11)-diene of formula (V) is reacted with hydrogen peroxide in a mixture of pyridine and dichloromethane in the presence of hexachloroacetone by known method, vii) the obtained 3,3,20,20-bis(ethylene-dioxy)-17a-hydroxy-5,10-epoxy-19-norpregn-9(11)-ene of formula (IV), containing approximately a 1:1 mixture of 5a,10a- and 5ss,10ss-epoxides, is isolated from the solution and reacted with a Grignard reagent obtained from 4-bromo-N,N-dimethyl-aniline in tetrahydrofuran.
Owner:RICHTER GEDEON NYRT

Method for preparing acid-proof polysulfonamide nanofiltration composite film

ActiveCN102120149ANo low separabilityNot low permeabilitySemi-permeable membranesSulfonyl chlorideComposite film
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.
Owner:HANGZHOU FANGRAN MEMBRANE TECH

Graphene material modified by water-soluble anthraquinone compound and preparation method of graphene material

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.
Owner:DALIAN UNIV OF TECH

Polysulfonamide nanofiltration or reverse-osmosis composite membrane, and preparation method thereof

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.
Owner:青岛致用新材料科技有限公司

Method for synthesizing and purifying Fasudil hydrochloride

InactiveCN102020636AReduce generationSolve excessive residualOrganic chemistryBenzodiazepineSodium bicarbonate
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%.
Owner:JIANGSU WANBANG BIOPHARMLS +1

Synthetic process of 1-chloro-cyclopropanecarbonyl chloride

ActiveCN104292089ASmooth process connectionReduce unit operationsOrganic compound preparationPreparation from heterocyclic compoundsSulfonyl chlorideChloride
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.
Owner:DALIAN JOIN KING FINE CHEM CO LTD

Process for the preparation of N-([1,2,4]triazolopyrimidin-2-yl)aryl sulfonamides

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.
Owner:CORTEVA AGRISCIENCE LLC

Methods for producing perfluoroalkanedi(sulfonyl chloride)

Novel methods for preparing perfluoroalkanedi(sulfonyl chloride) are disclosed as are uses for these compounds. In one aspect, a method comprising reacting dibromoperfluoroalkane with Na2S2O4 followed by treating with chlorine, an organic compound, and then chlorine to form perfluoroalkanedi(sulfonyl chloride) is provided. Novel perfluoroalkanedi(sulfonyl bromide) compounds are also disclosed.
Owner:UBE IND LTD

Vinylene carbonate preparation method

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.
Owner:RONGCHENG QINGMU CHEM MATERIALS

Preparation method of porous inorganic filling materials-fixed quinone compound

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.
Owner:DALIAN UNIV OF TECH

Method for preparing ethylene sulfate

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.
Owner:武汉松石科技股份有限公司

Fasudil hydrochloride compound and novel method thereof

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.
Owner:HAINAN LINGKANG PHARMA CO LTD

Production technology of phenyl sulfuryl chloride

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.
Owner:江苏康祥实业集团有限公司

Synthesis and preparation method of fasudil hydrochloride

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.
Owner:NOWA PHARMA

Cannabinoid crystalline derivatives and process of cannabinoid purification

Δ9 tetrahydrocannabinol (THC) esters comprising the reaction product of THC with at least one aryl sulfonyl chloride in the presence of at least one tertiary amine. The resulting aryl sulfonic THC esters are highly crystalline and stable at room temperature in air, allowing for indefinite storage. The aryl sulfonic THC esters can be recrystallized for purification, and then hydrolyzed to recover the purified THC.
Owner:PRAIRIE PLANT SYSTEMS

Water-soluble high molecule intercalating agent containing thiourea group and preparation method

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.
Owner:TIANJIN YIMING ENVIRONMENTAL TECH CO LTD

Synthesis method of ibrutinib

The invention discloses a synthesis method of ibrutinib. The method uses Suzuki coupling reaction and Kumada coupling reaction, does not need to separate the intermediate, obtains the intermediate (9) at high yield by a one-pot process, and uses mixed anhydrides instead of acryloyl chloride. The technique utilizes cheap 4-halodianisole as the initial raw material, adopts Suzuki coupling reaction and Kumada coupling reaction, and uses the one-pot process. The whole route is disclosed in the specification. The method can obtain the intermediate (9) (the chemical purity and optical purity are greater than or equal to 99%) at high yield without separating and purifying the intermediate, and avoids microwave, high temperature / high pressure and other specific reaction conditions; and the acrylic acid and mixed anhydrides generated by acyl chloride and sulfonyl chloride are used instead of the acryloyl chloride in the last step to avoid the amidation reaction of the intermediate (10) in multiple sites and reduce the generation of the byproduct, thereby obtaining the high-purity ibrutinib at high yield. The method has the advantages of short process route and lower cost, and is beneficial to the environment and suitable for industrialized scale-up production.
Owner:ARROMAX PHARMATECH

An ultraviolet positive photoresist

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.
Owner:XILONG SCI CO LTD

Organosilicon water-proof emulsion for building surface and preparation thereof

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.
Owner:宁君 +1

Synthetic method and application of porphyrin type near-infrared sulfur ion fluorescence probe

The invention discloses a synthetic method and application of a porphyrin type near-infrared sulfur ion fluorescence probe. The fluorescence probe is prepared by reaction of TPP-OH and 2,4-dinitrobenzene sulfonyl chloride as raw materials, N,N-DIEA as a catalyst and dichloromethane as a solvent at room temperature. The probe can carry out fluorescence detection of high sensitivity and selectivity on sulfur ions. Compared with an existing small organic molecule fluorescence probe, the obtained fluorescence probe has longer fluorescence emission wavelength (lambda em > 650 nm), can carry out detection of high sensitivity, selectivity and timeliness on the micro sulfur ions on a near infrared region, and has huge application prospects in the biological and environment detection field.
Owner:HUNAN UNIV OF SCI & TECH

Aromatic polymer sulfonamide, and preparation method and application thereof

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.
Owner:NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI

Preparation method of S-aryl phosphorothioate

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.
Owner:ZHENGZHOU UNIV

Preparation method of fasudil hydrochloride

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.
Owner:CHENGDU XINJIE HIGH TECH DEV CO LTD

Preparation method of porous inorganic filling materials-fixed quinone compound

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, sothat 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.
Owner:DALIAN UNIV OF TECH

Preparation method of trifluoro methanesulfonic anhydride

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%.
Owner:JIANGXI GUOHUA IND CO LTD

Guanidinylation SS-PAAs polymer as well as preparation and application thereof

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.
Owner:SHENYANG PHARMA UNIVERSITY

Method for synthesizing p-acetamido benzene sulfonyl chloride by phosphorus pentachloride

The invention relates to a method for synthesizing p-acetamido benzene sulfonyl chloride by phosphorus pentachloride, relating to the preparation method for sterilization and mould inhibition midbody of sulfonamides. The invention takes acetanilide and chlorosulfonic acid as raw materials, uses phosphorus pentachloride as chlorinating agent; under the action of organic dissolvent, the raw materials are sulfonated, chloridized, separated, and washed to obtain the product. The invention has the effects of little chlorosulfonic acid usage, high product yield, few generated waste acid,, completely cycling dissolvent, recycled by-products, low manufacturing cost, being convenient to popularize and apply, and the like. The products prepared by the method can be widely applied to the preparation of the sterilization and mould inhibition of sulfonamides and industries such as coating, plastics, pesticides, etc.
Owner:CHONGQING UNIV

Synthetic method of deuterium-marked sulfanilamide

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.
Owner:SHANGHAI RES INST OF CHEM IND

Method for catalyzed synthesis of high-purity 4-chloromethyl-5-methyl-1,3-dioxol-2-one

The invention discloses a method for catalyzed synthesis of high-purity 4-chloromethyl-5-methyl-1,3-dioxol-2-one. The method comprises the following steps: reacting 4,5-dimethyl-1,3-dioxol-2-one as a raw material with sulfonyl chloride as a chlorination reagent for 1-5 hours in an organic solvent under the effect of a catalyst; evaporating to remove the solvent after the reaction is ended, so as to obtain the target product 4-chloromethyl-5-methyl-1,3-dioxol-2-one. The preparation method disclosed by the invention is high in selectivity, one-step in reaction, free of by-product, high in reaction yield, safe and reliable to produce, simple to operate, low in production cost, and fewer in three wastes, and has great implement value and socioeconomic benefits.
Owner:HEFEI UNIV OF TECH
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