424 results about "Methylaniline" patented technology

The invention concretely relates to a synthetic technology for pyraclostrobin. The synthetic technology comprises: firstly performing cyclization to obtain 1-(4-chlorophenyl)-pyrazol-3-one, oxidizing the pyrazol ring under the effect of an oxidant to generate 1-(4-chlorophenyl)-3-hydroxypyrazole, then using 2-nitrobenzyl bromide to performing etherification to generate 1-(4-chlorophenyl)-3-[2-(nitrophenyl)methoxy]-1H-pyrazole, then using a reducing agent to perform nitro reducing, so as to generate N-hydroxyl-2-[N'-(4-chlorophenyl)pyrazol-3'-yloxymethyl]aniline, then using ClCO2CH3 to perform N-acylation reaction to generate methyl N-hydroxyl-N-2-{[N'-(4-chlorophenyl)pyrazol-3'-yloxymethyl]phenyl}formate, and finally performing hydroxyl methylation under an alkaline condition to generate pyraclostrobin. The technology enables all operations in the pyraclostrobin preparation process to be relatively controllable, helps to improve the stability of the preparation process and improve the product yield, successfully employs low-cost reagents and substantially reduces production cost, and also the employed reagents are relatively small in toxicity, is relatively beneficial for environment protection, and has no corrosivity on plastic pipes, so that the production safety is improved.

The present invention relates to a preparation method of pinoxaden, the steps are as follows: 2,6-diethyl-4-methylaniline is reacted with sandmeyer to obtain 2,6-diethyl-4-methylbromobenzene, and then mixed with Malononitrile is coupled under the catalysis of cuprous iodide to obtain 2,6-di-ethyl-4-methylphenylmalononitrile, and finally hydrolyzed in hydrogen peroxide solution to obtain 2,6-diethyl-4 ‑Methylphenylmalonamide; subsequent reaction with [1,4,5]‑oxadiazepine dihydrobromide in the presence of triethylamine to give 8‑(2,6‑diethyl‑ 4-methylbenzene)tetrahydropyrazol[1,2d][1,4,5]-oxadiazepine-7,9-dione, preferably reacted with pivaloyl chloride to obtain pinoxaden. The invention adopts a low-priced catalyst to reduce the production cost, and in addition, hydrogen peroxide-alkali is used as the hydrolysis system in the preparation process, which greatly reduces environmental pollution.

The invention provides a method for preparing bromhexine hydrochloride, which comprises the steps as follows: (1) 2-amino-3,5-dibromo benzaldehyde and reducing agents are in a reduction reaction to generate 2-amino-3,5-dibromo benzyl alcohol; (2) 2-amino-3, 5-dibromo benzyl alcohol that is obtained in the step (1) reacts with chlorinating agents to generate 2, 4-bromine-6-chloride methylaniline; and (3) 2,4-bromine-6-chloride methylaniline obtained in the step (2) and N-methylcyclohexylamine are in an amination reaction, and then 2, 4-bromine-6-chloride methylaniline and HCl salification agents are in a salification reaction, so that bromhexine hydrochloride is obtained. The preparation method adopts multiple advanced technologies, is easy to get starting materials, and has the advantages of stable property of intermediates, extremely low environment pollution, high yield coefficient of products and high purity.

The invention provides a preparation method and application of an anti-soil polymer. The prepared polymer is used as a dispersant for a hydraulic cementing agent and/or an aqueous dispersion for potential hydraulic cementing agent and has good anti-soil performance. The preparation method the anti-soil polymer comprises a step of subjecting polyether macromonomer A with a special structure, monomer B containing a phosphoric acid or phosphorous acid group, optional monomer D and aldehyde C to condensation polymerization so as to prepare the anti-soil polymer, wherein the monomer D is selected from the group consisting of phenol, aniline, p-/o-aminobezene solfonic acid, p-/o-hydroxybenzoic acid, p-/o-aminobenzoic acid, p-/o-hydroxyezene solfonic acid, p-/o-toluidine and p-/o-methylphenol, a mol ratio of the polyether macromonomer A to the monomer B to the monomer D is 1: (0.5-12): (0-8.0), and a mol ratio of the polyether macromonomer A to the monomer B and the monomer D is 1: (0.5-12.0).

The invention discloses a serum creatinine detecting reagent, and belongs to the technical field of clinical in-vitro detection. According to the serum creatinine detecting reagent, gamma-Fe2O3 nano-particles are added into a reagent R1, so that the activity of peroxidase and the specificity to a substrate are enhanced, and the interferences of reducing substances, such as ascorbic acid, uric acid, glutathione and bilirubin, are reduced; meanwhile, the gamma-Fe2O3 nano-particles also serve as a catalyst of a reaction; the interference of endogenous creatine is effectively eliminated by the combination action of the gamma-Fe2O3 nano-particles and the peroxidase. In addition, the serum creatinine detecting reagent adopts N-ethyl-N-(2-hydroxy-3-sulfonated propyl)-3-methylaniline sodium salt (TOOS) as a chromogen, so that the reagent is more stable; the analysis sensitivity is high. The substances, such as lipase and lipoprotein lipase, are also added into the reagent R1, so that the influence of lipid turbidity can be removed effectively; therefore, the reagent of the invention has higher anti-jamming capability and stability.

The invention discloses a synthesis method of pinoxaden, and belongs to the field of chemical engineering. The method comprises the following steps that 2,6-diethyl-4-methylaniline is subjected to sodium nitrite diazotization and thermal decomposition to generate 2,6-diethyl-4-methylbromobenzene; diethyl malonate is added into [1,4,5]-oxadiazepine dihydrobromide hydrate and an alkaline catalyst tosynthesize dihydro-1H-pyrazolo[1,2-d][1,4,5]-oxadiaza-7,9(2H, 8H)-diketone, the dihydro-1H-pyrazolo[1,2-d][1,4,5]-oxadiaza-7,9(2H, 8H)-diketone and 2,6-diethyl-4-bromomethyl benzene are subjected tocoupling reaction to obtain 8-(2,6-diethyl-4-methyl phenyl)tetrahydropyrazolo[1,2-d][1,4,5]xazepine-7, 9(2H, 8H)-diketone; the 8-(2,6-diethyl-4-methyl phenyl)tetrahydropyrazolo[1,2-d][1,4,5]xazepine-7, 9(2H, 8H)-diketone is reacted with pivaloyl chloride to synthesize the final product pinoxaden. According to the synthesis method of the pinoxaden, the synthesis steps are shortened, operation is simple and convenient, the cost is reduced, the economic efficiency is high, and environmental pollution is little.

The process of preparing glycidic amine type polyfunctional epoxy resin includes the following steps: 1. reaction between 4, 4'-methylene di-o-methylaniline and chloroepoxy propane in the molar ratio of 1 to 4-20 in water-alcohol solvent at 40-90 deg.c for 3-10 hr; and 2. dropping water solution of alkali metal hydroxide in the concentration of 20 % at 60 deg.c to produce desalting ring-closing reaction at 60-80 deg.c, extracting with extractant, water washing, separating, and vacuum volatizing to obtain N, N, N', N'-tetraglycidyl-4, 4'-methylene di-o-methylaniline. The present invention is one industrial process with simple operation, low cost, high product quality, high yield and less three wastes.

The invention provides a method for preparing lidocaine hydrochloride, and belongs to the technical field of anesthetic synthesis. The method comprises the following steps: by taking 2,6-xylenol as a raw material, Pd/C as a main catalyst and 2,6-dimethylcyclohexanone as a promoter, performing liquid phase amination with ammonia water at high temperature, thereby obtaining a midbody 2,6-dimethylaniline; enabling sodium methylate, 2,6-dimethylaniline and N,N-lignocaine methyl acetate as raw materials to react at 90-95 DEGC, distilling while reaction is performed to remove methanol till no methanol can be evaporated out, continuously reacting for 30 minutes, cooling to the room temperature, adding dichloroethane, washing with water, and leaving to stand to layer, thereby obtaining an organic layer, namely, a lidocaine based dichloroethane solution; further adding hydrochloric acid into the lidocaine based dichloroethane solution, adjusting the pH value to be 3.5-4 by using hydrogen chloride, adding activated carbon to reflux for 20-40 minutes, filtering, concentrating the filtrate, cooling, crystallizing, and dying, thereby obtaining lidocaine hydrochloride. The lidocaine hydrochloride prepared by using the method is simple in synthesis process and high in product purity, that is, the purity can be greater than 99%, and the total yield is greater than 84%.

The invention discloses a synthetic method for 2-methyl-3-trifluoromethyl phenylamine. The method comprises the following steps: 1) preparing 3-nitro-4-methyl benzenesulfonic acid; 2) preparing 3-nitro-4-methyl-5-bromobenzenesulfonic acid; 3) preparing 2-nitro-6-bromotoluene; 4) preparing 2-nitro-6-trichloromethyl toluene; 5) preparing 2-nitro-6-trifluoromethyl toluene; 6) preparing 2-methyl-3-trifluoromethyl phenylamine, that is, adding 5% palladium-charcoal and methanol in 2-nitro-6-trifluoromethyl toluene obtained in step 5), carrying out hydrogenation reduction at a temperature of 35 DEG C and removing a catalyst so as to obtain 2-methyl-3-trifluoromethyl phenylamine. According to the invention, p-toluenesulfonic acid is used as a starting material, and therefore, disadvantages of theprior art are overcome and yield of a target product is improved.

The invention provides a small and dense low-density lipoprotein cholesterin (sdLDL-C) detection kit which comprises double liquid reagents, including a reagent R1 and a reagent R2, wherein the reagent R1 comprises an MOPS buffer liquid (the pH value is 7.0), cholesterol esterase, cholesterol oxidase, phospholipase, catalase, polyoxyethylene alkyl phenyl ether (JK-14) as a surfactant A, polyoxyethylene benzyl styrene ether (A3PK) as a protecting agent, and N-ethyl-N-(2-hydroxyl-3-sulfopropyl)-3-methylaniline sodium salt (TOOS); the reagent R2 comprises an MOPS buffer liquid (the pH value is 7.0), peroxidase, polyethylene glycol octylphenol ether (Triton X-100) as a surfactant, 4-amino antipyrine (4-AA), and sodium azide. The method provided by the invention is high in sensitivity, high in specificity, simple in reagent preparation, free of sample pretreatment, and worthy of popularization and application.

The invention relates to a method for preparing 2-methyl-4-(1,1,1,2,3,3,3-heptafluoro-2-propyl) aniline which is obtained by reaction of 2-methylaniline with heptafluoro-2-bromopropane under the effect of an initiator. According to the method, the raw materials are low in cost, the reaction condition is mild, and the process is simple and accessible, so that the method is an ideal industrialized production method.

The invention belongs to the field of organic synthesis and relates to a method for preparing 3-chloro-4-methylaniline through catalytic hydrogenation. The method comprises the steps of using 3-chloro-4-methylnitrobenzene as raw material and alcohol or alcohol-water as solvent, and performing hydrogenation reduction at the presence of a two component Pd-Fe/C catalyst to obtain the final product. The obtained 3-chloro-4-methylaniline has a selectivity of over 99.9% and a yield of over 99%. The method for preparing 3-chloro-4-methylaniline provided by the invention has the advantages of simple process, mild operating condition, little pollution, and high activity and selectivity of the used catalyst, and can effectively reduce production costs compared with the traditional process. The catalyst used can be used repeatably.

The invention relates to a glycated albumin (GA) enzymatic detection kit, which comprises a GA reagent 1 and a GA reagent 2. The GA reagent 1 comprises tris(hydroxymethyl)aminomethane, aminoantipyrine (4-AAP), protease K, calcium acetate (CaAc2), potassium ferrocyanide trihydrate (K4Fe(CN)6.3H2O), copper acetate (CuAc2) and Cholic acid. The GA reagent 2 includes tris(hydroxymethyl)aminomethane, N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3-methylaniline sodium salt (TOOS), fructosaminase, Triton X-100 and peroxidase. The invention aims to provide the glycated albumin enzymatic detection kit and its detection method with the characteristics of strong specificity, high sensitivity, short time, simple operation mode, and accurate and reliable detection result.

The invention discloses a high-performance small and dense low-density lipoprotein cholesterol detection kit. The kit comprises the following raw materials in parts by weight; a reagent A: 90 to 110 mmol/L of a Good's buffer solution; 1-3 ku/L of cholesterol esterase, 1-2 ku/L of cholesterol oxidase, 0.7-0.9 ku/L of phospholipase, 400-600 ku/L of catalase, and 1-3 mmol/L N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3-methylaniline sodium salt (TOOS); and a reagent B: 90-110 mmol/L of the Good's buffer solution, 2-3 ku/L of peroxidase, 3-5 mmol/L of 4-aminoantipyrine and 0.04-0.06% of sodium azide. Theinvention relates to the technical field of lipoprotein cholesterol detection, and discloses the high-performance small and dense low-density lipoprotein cholesterol detection kit. The non-sdLDL-C components are removed through cholesterol lipase, cholesterol oxidase, phospholipase and catalase; the interference of other lipoprotein cholesterol on the detection process is avoided, the capacity ofthe small and dense low-density lipoprotein cholesterol in serum can be directly determined by using a full-automatic biochemical analyzer, and the kit is suitable for the requirements of clinical andlaboratory on the determination of the content of the small and dense low-density lipoprotein cholesterol.

The anti-knocking agent for gasoline is made up by using (by weight portion) alpha-methylaniline 46-81 portions, methyl tert-butyl ether (MTBE) 15-50 portions, toluene 2-4 portions, distilled gasoline 0.9-1.5 portions, raffinate oil 0.9-1.5 portions and 2,6-di-tert-butyl-p-cresol 0.1-0.6 portions and uniformly mixing them at plus or minus 35 deg.C and normal pressure. Said invented product can raise octane value of gasoline, and solve the knocking problem of gasoline when it is combusted.

The invention provides a gas chromatography-mass spectrometry detection method for a methylaniline compound. The method comprises the following steps of: A) extraction of a sample, namely adding an acid into the sample to extract the methylaniline compound into an acid liquor phase, adding alkaline into acid liquor phase extract to regulate pH to be neutral, adding methylene chloride to reextract the methylaniline compound in the neutral extract into the methylene chloride, and performing volume fixing to obtain a sample detection solution; and B) detection of the sample, namely separating the obtained sample detection solution by using a DB-1MS fused silica capillary column, and performing gas chromatography-mass spectrometry detection. The quantitative detection of the methylaniline compound is realized; the method is high in accuracy, low in detection limit, high in extraction efficiency and easy to operate, and can be widely applied to the detection of the methylaniline compound in a crude oil sample, a gasoline sample, a diesel sample and the like; the interference of other compounds in an extraction process can be eliminated; and powerful support can be provided for the environmental performance evaluation and monitoring of the sample.

The invention relates to the technical field of medical examination, and specifically relates to a triglyceride detecting kit. The kit comprises an agent R1 and an agent R2, wherein the agent R1 comprises glycerol kinase, lipoprotein lipase, peroxidase, composite chromogen and magnesium salt; the agent R2 comprises glycerophosphate oxidase, 4-ampyrone and triphosadenine; the composite chromogen comprises some of 3-methyl-N, N-aniline dipropyl sulfonate, N-ethyl-N-(3-sulfopropyl)-3-sodium methylaniline, N, N-bi(4-sulfobutyl)-3-methylaniline disodium salt, N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3-sodium methylaniline, and 2, 4, 6-tribromo-3-hydroxybenzoic acid. The kit in detecting of triglyceride is high in sensitivity, short in detecting time, and high in interference resistance.

The invention discloses a jet type membrane reactor and a method for preparing methylaniline by continuous catalytic hydrogenation. The jet type membrane reactor comprises a reactor body (1), a jet mixer (2) and a membrane assembly (3), wherein the jet mixer (2) is arranged at the top in the reactor body (1), the membrane assembly (3) is positioned below a discharging hole of the jet mixer (2) in the bottom in the reactor body (1), the jet mixer (2) is provided with a liquid phase feeding hole, a gas phase feeding hole and a circulating feeding hole, and a product discharging hole is formed in a place of the reactor body (1), which penetrates through the membrane assembly (3). The jet type membrane is compact in structure, small in occupation area and simple in process route, is reduced in energy consumption, and accords with the requirement of sustainable development.

The invention discloses a method for preparing lidocaine. The method comprises the following steps of: (1) by using 2, 6-dimethylnitrobenzene as a raw material, Pd/C as a catalyst and methanol as a solvent, carrying out reduction reaction with hydrogen at normal temperature and normal pressure to obtain an intermediate 2, 6-dimethylaniline; (2) reacting the obtained intermediate 2, 6-dimethylaniline with chloroacetyl chloride in the presence of potassium carbonate, and taking dichloromethane as a solvent to prepare an intermediate chloroacetyl-2, 6-dimethylaniline; and (3) reacting the obtained intermediate chloroacetyl-2, 6-dimethylaniline with diethylamine, taking normal hexane as a solvent, performing refluxing until the reaction is complete, performing washing with water and cooling toobtain lidocaine. The method disclosed by the invention is simple and convenient in technological process, few in operation links and relatively high in lidocaine yield, and the prepared lidocaine isgood in purity which reaches 99.5% or above, so that the method has a good industrial application prospect.

The invention discloses a method for preparing a pesticide intermediate 2,6-diethyl-4-methylphenyl bromide. The method comprises the following steps: preparing a first reactive raw material solution and a second reactive raw material solution; enabling the first reactive raw material solution and the second reactive raw material solution to carry out a diazo-reaction; adding the diazo-reaction solution into a denitrification reaction catalyst solution so as to carry out a denitrification reaction; distilling the denitrification reaction product to obtain distillate and waste liquor; extractingthe distillate to obtain the pesticide intermediate; and distilling and recycling the waste liquor. The first reactive raw material solution is a reactive mixed solution of 2,6-diethyl-4-methylaniline and hydrobromic acid, the second reactive raw material solution is a diazotization agent, and the concentration of the hydrobromic acid is 40-43%. According to the method disclosed by the invention,the yield and purity of the 2,6-diethyl-4-methylphenyl bromide are improved, and the production cost is reduced; and moreover, due to a distillation recovery manner, the waste hydrobromic acid is treated so as to be recycled, the raw material cost is reduced, and the environmental pollution caused by the waste hydrobromic acid is solved.

The invention discloses a method for catalyzing asymmetric hydrogenation of imines by an iridium/chiral diphosphine system, which comprises the following steps: reacting a chiral diphosphine ligand with a metal iridium precursor to prepare a complex in situ as a catalyst, and carrying out asymmetric hydrogenation on imines to prepare a chiral amine. The ligand is simple to prepare; catalyst dosage, simple operation, continuous operation can be realized, the preparation method is simple in process and suitable for large-scale preparation of chiral amine, the enantiomeric excess value of the product reaches 80% or above, and the preparation method has is excellent in effect when the S/C (2-ethyl-6-methylaniline/catalyst) rate is 500,000 during synthesis of the s-metolachlor intermediate, theyield reaches 95%, the enantioselectivity reaches 91%, and good industrial practicability is achieved.