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175 results about "Methylaniline" patented technology

Methylaniline may refer to: N-Methylaniline Toluidines 2-Methylaniline 3-Methylaniline 4-Methylaniline

Polymorphs of and synthetic process for an AZA-tetracyclic oxazepine inhibitor of KRAS-g12d

Provided herein are polymorphs and crystalline forms of 2-fluoro-5-((5S,5aS,6S,9R)-1-fluoro-12-(((2R,7aS)-2-fluorotetrahydro-1H-pyrrolizin-7a(5H)-yl)methoxy)-5-methyl-5a,6,7,8,9,10-hexahydro-5H-4-oxa-3,10a,11,13,14-pentaaza-6,9-methanonaphtho[1,8-ab]heptalen-2-yl)-3-methyl-4-(trifluoromethyl)aniline (Compound of Formula (I)), pharmaceutical compositions thereof, and methods of their use, for example, in the treatment of cancer. Also provided herein are synthetic processes for the manufacture of a compound of Formula (I) (i.e., 2-fluoro-5-((5S,5aS,6S,9R)-1-fluoro-12-(((2R,7aS)-2-fluorotetrahydro-1H-pyrrolizin-7a(5H)-yl)methoxy)-5-methyl-5a,6,7,8,9,10-hexahydro-5H-4-oxa-3,10a,11,13,14-pentaaza-6,9-methanonaphtho[1,8-ab]heptalen-2-yl)-3-methyl-4-(trifluoromethyl)aniline). Also provided are compounds useful in its synthesis (e.g., those of Formulae (A), (B), (By), and (H)) and synthetic processes directed thereto.
Owner:GENENTECH INC

Method and system for synthesizing N-methylaniline and co-producing N, N-dimethylaniline by gas phase method

The invention relates to a method and a system for synthesizing N-methylaniline and co-producing N, N-dimethylaniline by a gas phase method, and belongs to the technical field of chemical engineering. The system comprises a raw material gasification unit, a reaction unit, a separation and rectification unit and a hydrogen recovery unit which are connected through pipelines. The method comprises the following steps of: firstly, mainly synthesizing N-methylaniline from raw materials aniline and part of methanol in a first-methylaniline reactor, then partially or completely feeding first-methylaniline reaction gas into a second-methylaniline reactor, adding methanol steam, and further reacting to generate N, N-dimethylaniline. And after the product gas is subjected to heat exchange energy recovery, a liquid phase and a gas phase respectively enter the separation and rectification unit and the hydrogen recovery unit. The purification of N-methylaniline and N, N-dimethylaniline and the recovery of byproduct hydrogen are realized. The yield of N, N-dimethylaniline (in terms of aniline) can be adjusted in a range of 5-30% by adjusting reaction conditions and a feeding ratio.
Owner:SOUTHWEST RES & DESIGN INST OF CHEM IND

Preparation method of 2-fluoro-4-methylaniline

The invention discloses a preparation method of 2-fluoro-4-methylaniline, which has the following synthetic route: # imgabs0 #, wherein R1 is selected from one of-CN,-CX3 (wherein X is halogen) and-COOR (wherein R is H or C1-C6 alkyl). The synthesis method disclosed by the invention is simple, has the advantages of high yield, simple post-treatment, low cost and the like, meanwhile, the raw materials are easy to obtain, the reaction danger coefficient is low, the problems of high synthesis cost, low yield, high reaction danger coefficient and the like in the prior art are solved, and the method has a good industrial application prospect.
Owner:PAPANNA (BEIJING) TECH CO LTD

Catalyst for synthesizing N-methylaniline and preparation method thereof

The invention provides a catalyst for synthesizing N-methylaniline and a preparation method thereof, the catalyst comprises an active component, a carrier and an auxiliary agent, the active component comprises oxygen-containing compounds of copper, zinc and chromium, the carrier is gamma-alumina subjected to surface hydroxylation treatment, and the auxiliary agent is a cerium-molybdenum bimetallic alloy. The preparation method comprises the following steps: loading the active component on the hydroxylation carrier through ultrasonic impregnation, drying, further loading the cerium-molybdenum auxiliary agent, and carrying out reduction alloying and roasting activation to form the composite catalyst. The catalyst is a regular cylinder, has the diameter of 4-6mm and the length of 4-6mm, has an optimized pore structure and surface properties, and is suitable for methylation reaction of aniline and methanol. According to the method, the dispersity of active components is improved through modified chromic oxide, the mass transfer efficiency is enhanced through a hydroxylation carrier, the synergistic catalysis effect of cerium-molybdenum alloy is combined, the reaction activity and selectivity are remarkably improved, meanwhile, side reactions are inhibited, the stability is enhanced, and the method can be widely applied to industrial production of N-methylaniline.
Owner:AOLI PETROCHEMICAL CO LTD DONG FANG BRANCH

Preparation method of key intermediate of chlorantraniliprole

The invention provides a preparation method of a chlorantraniliprole key intermediate 2-amino-5-cyano-N, 3-dimethyl benzamide, which comprises the following steps: taking cheap and easily available o-methylaniline as a raw material, acylating an aniline substrate through Boc anhydride, carrying out ortho-lithiation on n-butyllithium, introducing carbon dioxide gas, and carrying out acid hydrolysis to obtain 2-amino-3-methyl benzoic acid, thereby obtaining the chlorantraniliprole key intermediate 2-amino-5-cyano-N, 3-dimethyl benzamide. The preparation method comprises the following steps: firstly, preparing an isatoic anhydride intermediate, then carrying out triphosgene ring closing to obtain an isatoic anhydride intermediate, carrying out bromine para-position halogenation, carrying out cuprous cyanide high-temperature Rosenmn-von Braun reaction, and finally carrying out methylamine ring opening to obtain the target product 2-amino-5-cyano-N, 3-dimethylbenzamide, and although the route is long, the yield is high, the continuity is good, few industrial three wastes are generated, and the cost is lower, so that the preparation method has great industrial production value.
Owner:SHANDONG LONGXI PLANT PROTECTION CO LTD

Method for extracting and separating N-methylaniline and N, N-dimethylaniline

The invention discloses a method for extracting and separating N-methylaniline and N, N-dimethylaniline, and relates to the technical field of organic compound separation.The method comprises the steps that a reaction product of aniline and methyl alcohol is taken and fed into an adsorption refiner to be adsorbed, and a mixture A is obtained; feeding the mixture A into a light component removal tower for light component removal, collecting at the top of the light component removal tower to obtain light components, feeding the light component removal tower into a heavy component removal tower for heavy component removal, and collecting at the top of the heavy component removal tower to obtain a mixture B; taking the mixture B, feeding from the middle part of an extractive distillation tower, taking an extracting agent, feeding from the upper part of the extractive distillation tower, and performing extractive distillation; collecting the N, N-dimethylaniline at the top of the extractive distillation tower to obtain N, N-dimethylaniline, and collecting the N, N-dimethylaniline at the bottom of the extractive distillation tower to obtain an N-methylaniline mixed solution; feeding the N-methylaniline mixed solution into a desorption tower for desorption; collecting at the top of the desorption tower to obtain N-methylaniline, and collecting at the bottom of the desorption tower to obtain the extracting agent.
Owner:CHANGZHOU JIANGYE INFORMATION ENG TECH CO LTD

Electrochemical synthesis method of 4 '-N-methylbenzyl-3-indole derivative

The invention relates to the field of chemical synthesis, in particular to an electrochemical synthesis method of a 4 '-N-methylbenzyl-3-indole derivative. According to the preparation method, selected electrons are traceless oxidizing agents, the energy conversion rate is high, no catalyst is needed in the reaction, the reaction steps are few, raw materials are easy to obtain, the reaction conditions are mild, operation is easy, convenient and safe, the substrate expansion range is wide, the compound functional group tolerance is high, the product yield can reach 80% or above, and the compound can be prepared in a gram level. N-methyl N-alkylaniline or N-methylaniline is used for carrying out electrochemical oxidation reaction on indole, N-methyl provides methylene to realize connection between benzene ring para-positions of the N-methyl N-alkylaniline and N-methylaniline and the C3 position of indole, and then the 3-arylmethylindole derivative is efficiently synthesized.
Owner:SHENZHEN POLYTECHNIC

Non-noble metal catalyst Cu / TiO2-P25, preparation method thereof and application of non-noble metal catalyst Cu / TiO2-P25 in synthesis of N, N-dimethyl-p-toluidine in heterogeneous system

The invention relates to a non-noble metal catalyst Cu / TiO2-P25, a preparation method thereof and application of the non-noble metal catalyst Cu / TiO2-P25 in synthesis of N, N-dimethyl-p-toluidine from formaldehyde and N-methylaniline, and belongs to the field of catalysts. According to the catalyst, copper nitrate trihydrate serves as a copper source, P25 type TiO2 serves as a carrier, metal is loaded on the P25 type TiO2 through a deposition-precipitation method, the catalyst Cu / TiO2-P25 is obtained through hydrogen reduction in a tubular furnace, then the catalyst Cu / TiO2-P25 is dispersed in a solvent, and hydrogen serves as a hydrogen source to catalyze formaldehyde and N-methylaniline to synthesize N, N-dimethyl p-toluidine. Wherein the Cu / TiO2-P25 catalyst with the copper content of 6% has excellent catalytic performance, and when the hydrogen pressure is 3.5 MPa, the temperature is 180 DEG C and the reaction is performed for 8 hours, the conversion rate of N-methylaniline reaches 100%, and the selectivity on N, N-dimethyl-p-toluidine is 50.8%. The preparation method is simple and low in production cost, is used for catalyzing formaldehyde and N-methylaniline to synthesize N, N-dimethyl-p-toluidine, and has a wide industrialization prospect.
Owner:ANHUI UNIV

Preparation method of N-methylaniline

PendingCN119638577Areduce the effectThe reaction process is green and environmentally friendlyOrganic compound preparationAmino compound preparationMethylanilinePtru catalyst
The invention provides a preparation method of N-methylaniline, and relates to the technical field of synthesis of N-methylaniline. The fixed bed reactor is adopted, under the condition that the specific catalyst exists, aniline, carbon dioxide, carbon monoxide and hydrogen are mixed and react to prepare N-methylaniline, the final conversion rate of aniline can reach 98% or above, and the N-methylaniline product yield is high.
Owner:LANZHOU UNIV

Method and system for comprehensively utilizing aqueous phase in aniline methylation reaction product

The invention discloses a method and system for comprehensively utilizing a water phase in an aniline methylation reaction product, and the method comprises the following steps: firstly, taking the water phase in the aniline methylation reaction product as a raw material, and rectifying the raw material to obtain a methanol distillate and a mixed solution containing aniline, N-methylaniline, trace N, N-dimethylaniline organic matters and water; a low-boiling-point aromatic hydrocarbon solvent is used as an extraction agent, the obtained mixed solution is used as a raw material, and the raw material and the extraction agent are subjected to multiple times of reverse contact for extraction; standing and layering to obtain an extraction phase and a raffinate phase; wherein the extraction phase is a mixture of an amine organic matter and an extraction agent, and the raffinate phase contains wastewater with the content of the amine organic matter reduced. According to the method, the methanol, the amine mixed organic matters and the extraction agent can be recycled, the content of the organic matters in the water can be remarkably reduced, the water can be discharged after reaching the standard after being subjected to further biochemical treatment, and the resource comprehensive utilization of the water phase solution is realized.
Owner:JIANGSU YANJIANG CHEM RESOURCES DEV RES INST CO LTD +1

Method for synthesizing chlorfenapyr bisamide intermediate by one-pot method

The invention discloses a method for synthesizing a chlorfenapyr bisamide intermediate by a one-pot method, which comprises the following steps: by taking aniline as an initial raw material, reacting the aniline with 2-bromoheptafluoropropane under the action of a catalyst and an acid-binding agent to generate 4-heptafluoroisopropylaniline, distilling to recover excessive 2-bromoheptafluoropropane after the aniline is completely converted, and separating the 2-bromoheptafluoropropane from the 4-heptafluoroisopropylaniline to obtain the chlorfenapyr bisamide intermediate. Adding bromotrifluoromethane into the reaction liquid to react to obtain 2-trifluoromethyl-4-(heptafluoroisopropyl) aniline, then carrying out oxidation-reduction reaction on the dropped hydrogen peroxide and excessive sodium hydrosulfite, and after the sodium hydrosulfite is completely consumed, reacting to obtain 2-trifluoromethyl-4-(heptafluoroisopropyl) aniline; and carrying out benzene ring bromination reaction on dropwise added hydrogen peroxide, the brominating agent in the reaction liquid and the 2-trifluoromethyl-4-(heptafluoroisopropyl) aniline to obtain the 2-bromo-4-(heptafluoroisopropyl)-6-(trifluoromethyl) aniline, wherein the brominating agent in the reaction liquid and the 2-trifluoromethyl-4-(heptafluoroisopropyl)-6-(trifluoromethyl) aniline are subjected to benzene ring bromination reaction. The method is simple in process, high in yield, low in raw material cost and suitable for industrial production.
Owner:湖南速博生物技术有限公司

Secondary gas-phase quenching reactor for producing N-methylaniline

The utility model discloses a two-stage gas-phase quenching reactor for producing N-methylaniline, which comprises a first-stage reactor, a second-stage reactor and internal parts which are arranged as a whole and are inseparable. Therefore, the alcohol-amine ratio (the molar ratio of methanol to aniline) of the second-stage gas-phase quenching reactor is adjustable, the mixed material is uniformly distributed, and the methanol and the aniline are subjected to high-selectivity reaction. The second-stage reactors are tubular reactors, a three-stage mixing distributor for methanol and materials is arranged at a first-stage inlet, initial distribution of the materials is provided, and uniform mixing of methanol and main materials is adjusted. An annular calandria type quenching methanol distributor is arranged between the secondary reactors, and distribution nozzles are uniformly arranged on the whole circumferential surface. The shell side of the reactor adopts heat transfer oil for heat transfer, and an annular baffle plate is arranged in the reactor. The two-stage reactor is provided with a double-tube-plate structure, so that the influence on the product purity caused by entering a reaction product after a small amount of heat-conducting oil leaks is prevented.
Owner:JIANGSU OULIKE ENVIRONMENTAL PROTECTION TECH CO LTD

Synthesis process of N-methylaniline

The invention belongs to the technical field of organic synthetic chemistry, and particularly relates to a synthesis process of N-methylaniline. By adopting the special biomass porous carbon loaded nickel-copper bimetallic catalyst, the selectivity and the conversion rate of the reaction are improved, and the generation of byproducts is reduced, so that the burden of subsequent separation is reduced, the utilization rate of the raw materials is improved, and the yield is increased by introducing the micro-channel reactor and combining a microwave heating technology. Compared with the prior art, the method has the advantages that the mixing efficiency and the heat mass transfer rate of materials are improved, the reaction time is shortened, in the separation and purification process, a membrane separation and rectification combined technology and an efficient phase splitter are adopted, salt water is not needed, salt-containing wastewater is avoided, meanwhile, the recovery efficiency of methanol and aniline is improved, and cyclic utilization of a solvent is achieved. The whole process reduces the energy consumption, improves the production efficiency, reduces the emission of pollutants and meets the requirements of green chemistry through waste heat recovery, heating mode optimization and separation process.
Owner:SUZHOU HENGCHANG BIOTECHNOLOGY CO LTD

Basic cupric carbonate-based composite catalyst for synthesizing N-methylaniline through N methylation of aniline and preparation method of basic cupric carbonate-based composite catalyst

The invention relates to the technical field of catalysts for synthesizing N-methylaniline, in particular to a basic cupric carbonate based composite catalyst for synthesizing N-methylaniline through N methylation of aniline and a preparation method of the basic cupric carbonate based composite catalyst. The selectivity of a conventional copper-based catalyst to N-methylaniline in a reaction for preparing N-methylaniline through N methylation of aniline is difficult to reach 90% or above. Aiming at the technical problem, the invention provides the basic cupric carbonate-based composite catalyst for synthesizing N-methylaniline through N methylation of aniline, the structural formula of the basic cupric carbonate-based composite catalyst can be represented as CuM (OH) x (CO3) y, M in the structural general formula comprises one or more of metal elements of zinc, aluminum, chromium, lanthanum and manganese, and by optimizing the composition of the metal elements in the catalyst and the pH value in the coprecipitation process, the N-methylaniline can be synthesized. The basic cupric carbonate-based composite catalyst with a relatively good catalytic effect is obtained, and obvious inactivation is not found when the basic cupric carbonate-based composite catalyst can stably and continuously run for 1000 hours under the condition of keeping a relatively high N-methylaniline yield.
Owner:JIANGSU JINGYING NEW MATERIALS CO LTD

A process, apparatus, catalyst and method of preparation for removing meta-toluidine and indole from coking nanofiltration concentrated water

The application provides a process and equipment for removing m-methylaniline and indole in coking nanofiltration concentrated water, a catalyst and a preparation method thereof, and the water quality of the coking nanofiltration concentrated water is as follows: conductivity 21300-34560 muS / cm, sulfate ion 567-1340 mg / L, m-methylaniline 45-78 mu g / L, and indole 23-39 mu g / L; the process comprises the following treatment steps: the coking nanofiltration concentrated water enters the ozone catalytic tower from the bottom of the tower and flows out from bottom to top, and the ozone catalytic tower is internally provided with a modified peanut shell biochar catalyst; after the ozone catalytic reaction, the water quality of the coking nanofiltration concentrated water is as follows: conductivity 21300-34560 muS / cm, sulfate ion 567-1340 mg / L, m-methylaniline 3-7 mu g / L, and indole 1-6 mu g / L.
Owner:BAOSHAN IRON & STEEL CO LTD

A catalyst for preparing methylaniline, a preparation method and application thereof

ActiveCN121060526BMethylanilinePtru catalyst
The application discloses a catalyst for preparing methylaniline and a preparation method and application thereof, and belongs to the technical field of catalysts. The catalyst is prepared by modifying an activated carbon carrier with zirconium, cerium or nickel, treating the carrier with high-temperature nitrogen, loading active components Pd and pH-responsive polymers, solving the problems of low dispersion of the active components, easy poisoning and activity attenuation, and having good pH responsiveness and environmental adaptability. The preparation method optimizes a carrier modification process, adopts an impregnation method combined with timed stirring, controls reaction parameters, improves catalyst performance, realizes high selectivity and high yield of methylaniline, and has the advantages of high selectivity of the catalyst for methylaniline, inhibition of side reactions, adoption of a fixed bed reactor, simplification of operation, reduction of safety hazards, efficient reaction at a lower reaction temperature and pressure, and reduction of energy consumption and production cost.
Owner:XI AN JIAOTONG UNIV +1

A method for improving the quality of 2,6-dichloro-4-trifluoromethylaniline

The present invention relates to a method for separating and purifying a pesticide chemical product, in particular to a method for improving the quality of 2,6-dichloro-4-trifluoromethylaniline. First, a composite protective agent is added to the crude product of 2,6-dichloro-4-trifluoromethylaniline, and after mixing evenly, it is sent to a rectification device for vacuum rectification. The refined product of 2,6-dichloro-4-trifluoromethylaniline is obtained by rectification. The composite protective agent includes metal fluoride and amine compounds, which can inhibit the dechlorination of 2,6-dichloro-4-trifluoromethylaniline, greatly reduce the generation of impurities, and greatly improve the rectification yield of 2,6-dichloro-4-trifluoromethylaniline.
Owner:NANTONG DONGCHANG CHEM IND CO LTD

Method for reducing by-product N-methylaniline in RT base condensation liquid

The invention discloses a method for reducing by-product N-methylaniline in RT base condensation liquid. According to the method, potassium hydroxide modified activated carbon is added in condensation reaction. The potassium hydroxide modified activated carbon greatly reduces the generation of a by-product N-methylaniline in a condensation reaction, reduces the absorption of carbon dioxide in air by system materials, slows down the increase of tetramethyl carbonate, prolongs the catalytic life of tetramethyl ammonium hydroxide, saves the cost of raw materials, and has a good application prospect.
Owner:CHINA PETROLEUM & CHEMICAL CORP +2

Synthesis method of atavapam

The invention provides a synthesis method of atavapam, which comprises the following steps: carrying out nucleophilic addition-elimination reaction on commercially available raw materials and 4-methyl-3-trifluoromethylaniline under alkaline conditions, carrying out Suzuki coupling reaction under the action of a catalyst, carrying out pressurized hydrogenation, and carrying out chiral resolution, thereby obtaining the atavapam. And condensing with 2-fluoro-6-methyl benzoyl chloride under an alkaline condition, and further removing a Boc protecting group under an acidic condition to finish synthesis of the atavapam. According to the invention, a convergent synthesis process is adopted, tedious synthesis steps in the original process are shortened, and post-treatment is simpler and more controllable.
Owner:HANGZHOU NUOAO BIOMEDICAL TECH CO LTD

A method and system for co-producing N-methylaniline and N-methylindole

The present invention provides a method and system for co-producing N-methylaniline and N-methylindole. The method comprises: a first Cu-based catalyst catalyzes a first reaction between aniline and methanol to obtain a first gaseous mixed system containing N-methylaniline; ethylene glycol is introduced into the first gaseous mixed system, and part of the N-methylaniline and ethylene glycol in the first gaseous mixed system undergo a second reaction under the catalysis of a second Cu-based catalyst to be converted into N-methylindole, and finally a second gaseous mixed system containing N-methylaniline and N-methylindole is obtained; the second gaseous mixed system is condensed, flashed and distilled to separate N-methylaniline and N-methylindole. In the co-production method provided by the present invention, by means of a two-stage reaction, not only N-methylaniline is synthesized with high efficiency and low cost, but also co-production of N-methylaniline and N-methylindole is achieved.
Owner:SHAANXI HYDROGEN ENERGY TECH CO LTD

Zinc-silver battery electrolyte additive, zinc-silver battery electrolyte and zinc-silver secondary battery

The invention relates to the technical field of zinc-silver batteries, in particular to a zinc-silver battery electrolyte additive, a zinc-silver battery electrolyte and a zinc-silver secondary battery. A trace amount of negatively-charged surfactant N-ethyl-N-(3-sulfopropyl)-3-methylaniline sodium salt is added into the traditional KOH electrolyte of the zinc-silver secondary battery, and the problem of deformation of a zinc negative electrode caused by the existence of a free-state charge-discharge intermediate product Zn (OH) 4 < 2-> is inhibited by utilizing specific adsorption of amphoteric molecules and a negatively-charged functional group. The additive not only can stabilize the zinc negative electrode structure and improve the cycle performance of the zinc-silver battery, but also can enable the active substances in the zinc-silver battery to give full play to the capacity, and prolongs the service life of the zinc-silver secondary battery for repeated and stable discharge and energy supply.
Owner:NANKAI UNIV

Preparation process of 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid

The invention discloses a preparation process of 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid, and relates to the technical field of preparation of inorganic compounds. The invention relates to a preparation process of 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid, which comprises the following steps: reacting 3-chloro-2-methylaniline with hydrochloric acid and sodium methyl mercaptide to form an intermediate C1, reacting with acetyl chloride, catalyzing with anhydrous aluminum trichloride to form an intermediate C2, reacting with hydrogen peroxide and sodium hypochlorite to form an intermediate C4, and reacting with sodium chloride to form the 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid. The 2-chloro-4-(methylsulfonyl)-3-methyl benzoic acid is obtained after the reaction is completed.
Owner:SUQIAN KEYLAB BIOCHEMICAL CO LTD

Catalyst for preparing N-methylaniline through continuous catalysis of aniline as well as preparation method and application of catalyst

The invention provides a catalyst for preparing N-methylaniline through continuous catalysis of aniline as well as a preparation method and application of the catalyst, and relates to the technical field of synthesis of N-methylaniline. The catalyst is recorded as CuOx / CrOy / X, the catalyst is used in the process of preparing N-methylaniline through continuous catalysis of aniline, the problems of low conversion rate and selectivity of conversion from aniline to N-methylaniline through catalysis in the prior art are solved, and the final conversion rate of aniline and the selectivity of N-methylaniline can reach 99%.
Owner:LANZHOU UNIV

Process for the preparation of the intermediate of Tucatinib 4-([1,2,4]triazolo[1,5-a]pyridin-7-yloxy)-3-methylaniline

The application relates to the technical field of medicines, in particular to a preparation process of a Tucatinib intermediate 4-([1,2,4]triazolo[1,5-a]pyridin-7-yloxy)-3-methylaniline, which comprises the following steps: step 1: under a nitrogen atmosphere, a substitution reaction is carried out on a compound B and a compound C in a base and an organic solvent system to obtain a compound D; step 2: the compound D is added into a reduction catalytic solution system protected by nitrogen, after 8-30h of reaction at 70-120 DEG C, TLC tracking is carried out until the reaction is completed, 2-8 times the volume of the compound D is added into water, post-treatment and purification are carried out, and the compound A is obtained; wherein the reduction catalytic solution system comprises a reducing agent, a catalyst and an inorganic acid, the reducing agent comprises a reducing phosphoric acid, and the catalyst comprises iodine or a metal salt of iodine. The preparation process of the Tucatinib intermediate 4-([1,2,4]triazolo[1,5-a]pyridin-7-yloxy)-3-methylaniline in the application has mild reaction conditions, high product yield and high purity, the preparation process is environment-friendly, and can be used for industrial production.
Owner:SCINOPHARM CHANGSHU PHARMA

Three-channel colorimetric sensor for simultaneously detecting aflatoxin and precursor thereof as well as preparation method and application of three-channel colorimetric sensor

The invention relates to the technical field of harmful substance detection, in particular to a three-channel colorimetric sensor for simultaneously detecting aflatoxin and a precursor thereof as well as a preparation method and application of the three-channel colorimetric sensor. According to the method, COFFe / NiP-Ph is utilized for catalyzing 3, 3 ', 5, 5'-tetramethylbenzidine (TMB) to be oxidized to generate blue oxTMB, o-phenylenediamine (OPD) is utilized for generating yellow oxOPD, and then the aflatoxin and the precursor thereof are detected through a three-channel colorimetric sensor. Purple ox4-AT is generated by using a mixture of N-ethyl-N-(3-sulfopropyl)-3-methylaniline sodium and 4-aminoantipyrine (4-AT), so that the colorimetric response is realized in a short time. The preparation method of the COFFe / NiP-Ph nano enzyme comprises the following steps: 1, a synthesis process of Fe-TAPP; 2, synthesis of Ni-TAPP is carried out; and 3, synthesizing the iron / nickel porphyrin covalent organic framework. The colorimetric sensor can be prepared into a detection reagent or a kit so as to realize qualitative and quantitative detection of aflatoxin and a precursor thereof in a sample to be detected. The detection method is simple and convenient to operate, and complex pretreatment on a to-be-detected sample is not needed; the detection cost is low, the detection is quick, and the requirement on a detection instrument is low.
Owner:NANTONG UNIV

Method for analyzing purity of carbon black prepared from organic hazardous waste

The invention relates to the technical field of carbon black detection, in particular to a purity analysis method of carbon black prepared from organic hazardous waste. The purity analysis method comprises the following steps: S1, mixing carbon black with an organic amine solution to obtain a mixture; s2, mixing the mixture with an organic solvent, performing centrifugal filtration to obtain filtrate, and measuring the light transmittance; the organic amine comprises a mixed solvent of piperidine and N-methylaniline. The carbon black is prepared by the following method: (1) carrying out dehydration pretreatment on the organic hazardous waste, and crushing to obtain a particle sample; (2) pyrolyzing the particle sample under the inert gas condition at the pyrolysis temperature of 1100-1400 DEG C, separating out carbon black generated in the pyrolysis process along with a gas-phase product, and filtering and collecting by a filter membrane; and (3) cleaning the filter membrane with an organic solvent, filtering, and drying to obtain the carbon black. The purity analysis method is more accurate, and the analysis result can better represent the purity of the carbon black.
Owner:CHINESE RES ACAD OF ENVIRONMENTAL SCI

N-methylaniline impurity online spectrum monitoring device

The invention relates to the technical field of chemical monitoring, in particular to an N-methylaniline impurity online spectrum monitoring device which comprises a bottom rack, a plurality of glass boxes are evenly arranged on the bottom rack in the length direction, the glass boxes sequentially have different deflection angles, and the deflection angle difference values of the adjacent glass boxes are equal; by arranging the multi-angle deflection glass box, static and multi-angle static monitoring of N-methylaniline is realized, spectral characteristics of impurities in different directions can be effectively captured, and slow rotation of the glass box further drives the internal N-methylaniline to change angles, so that a light source can fully irradiate, and the detection accuracy is improved. Impurities possibly hidden due to local gathering are repeatedly exposed in dynamic rotation, a monitoring blind area is eliminated, the comprehensiveness of impurity detection is remarkably enhanced through the steps, and the accuracy of a monitoring result can be greatly improved especially for trace impurities which are not evenly distributed.
Owner:SHANDONG RONGHAI NEW MATERIALS TECHNOLOGY CO LTD

High adhesion asphalt anti-stripping agent and method of making same

This invention relates to the field of asphalt technology and discloses a high-adhesion asphalt anti-stripping agent and its preparation method; including the following steps: Step 1: Add amino-branched titanium dioxide to N-methylaniline and mix evenly to obtain a polyamine complex; Step 2: Mix terpene phenolic resin, methyl phenyl silicone resin, and additives evenly, add the polyamine complex and calcium hydroxide, and mix evenly to obtain a high-adhesion asphalt anti-stripping agent.
Owner:JIANGSU HIGH SPEED NEW MATERIAL TECH CO LTD

Ultrahigh-desalination and anti-oxidation reverse osmosis membrane and preparation method thereof

The preparation method comprises the following steps: step 1, first interfacial polymerization: immersing a polysulfone support membrane into a polyamine water phase solution, taking out the polysulfone support membrane, removing a solvent, immersing the polysulfone support membrane into an acyl chloride A part hydrolyzed oil phase solution, and carrying out first interfacial polymerization reaction, so as to obtain a polysulfone membrane; a nascent state reverse osmosis membrane is obtained; step 2, secondary interfacial polymerization: removing unreacted acyl chloride from the nascent state reverse osmosis membrane, then immersing the nascent state reverse osmosis membrane into an oil phase solution of acyl chloride B to carry out secondary interfacial polymerization reaction, and then carrying out heat treatment to obtain a reverse osmosis membrane semi-finished product; and step 3, third interfacial polymerization: immersing the semi-finished reverse osmosis membrane product into an oil phase solution of o-methylaniline, carrying out third interfacial polymerization, and carrying out heat treatment again to obtain the ultra-high-desalination and anti-oxidation reverse osmosis membrane. Under the condition of ensuring that the water flux is not greatly reduced, the ultra-high desalination rate of the reverse osmosis membrane is realized, and the service life of the membrane is prolonged.
Owner:NINGBO RXHL TECH CO LTD

1-pyrenecarboxaldehyde 4-(1, 2, 4-triazole-1-yl methyl) aniline Schiff base compound as well as preparation method and application thereof

The invention discloses a Schiff base compound generated by condensation of 1-pyrenecarboxaldehyde and 4-(1, 2, 4-triazole-1-yl methyl) aniline as well as a preparation method and application of the Schiff base compound. The Schiff base compound has certain fluorescence and anti-DPPH free radical activity, and has potential application value in preparation of fluorescent materials and antioxidants.
Owner:HUAIYIN TEACHERS COLLEGE