73 results about "Dibromopropane" patented technology

The invention discloses a method for preparing an antimicrobial polymer separation membrane, which comprises the following steps of: (1) selecting a polymer separation membrane containing a dimethylaminoethyl methacrylate surface modification layer as a basement membrane; and (2) soaking the basement membrane in aqueous solution of silver nitrate and aqueous solution of sodium borohydride in turn, taking out, soaking in cross-linking agent solution for quaternization and in-situ cross-linking reaction, taking out, cleaning, and drying to obtain the antimicrobial polymer separation membrane, wherein a reducing agent is sodium borohydride or sodium ascorbate; and a cross-linking agent is on ore more of alpha,alpha'-dichloro-p-xylen, 1,2-dibromoethane, 1,3-dibromopropane, and 1,4-dibromobutane. The polymer separation membrane prepared by the method fully utilizes the antibacterial performance of silver nanoparticles and quaternized dimethylaminoethyl methacrylate, and has excellent antimicrobial effect.

The invention discloses an immobilized pyridine quaternary ammonium salt halamine precursor I as well as a synthesis method and application thereof. The synthesis method comprises the following steps: preparing a compound III from 5,5-dimethyl hydantoin, dibromopropane and hydroxypyridine which serve as raw materials, and then carrying out backflow reaction with gamma-chloro(bromo, iodo) propyl triethoxy silane in acetonitrile for 7 to 48 hours to obtain an antimicrobial compound precursor I. The application of an antimicrobial in an antibacterial material comprises the following steps: preparing 1 to 5 percent by weight of a halamine precursor solution, modifying the surface of the material in an immobilized manner, and performing chlorination to obtain the antibacterial material. The synthesis method disclosed by the invention is easy to operate; with the introduction of a pyridine quaternary ammonium salt unit, the water solubility of the antibacterial agent is enhanced, and the use of an organic solvent in the preparation process of the antibacterial material is reduced. An antibacterial experiment shows that the prepared antibacterial material is relatively high in bactericidal activity against Gram-negative bacteria (E.coli ATCC25922) and Gram-positive bacteria (S.aureus ATCC25923). A formula is shown in the specification, wherein R is selected from Cl, Br or I, and n is an integer from 2 to 12.

The invention discloses bridge-linked acridine dimer and a preparation method and application thereof. The bridge-linked acridine dimer has the molecular formula of C29H24N4 and the structural formula which is shown in the description. The bridge-linked acridine dimer is prepared by the following steps: using 9-aminoacridine as an initial reactant, stirring and refluxing the 9-aminoacridine together with 1, 3-dibromopropane in an organic solvent, stirring and refluxing the recrystallized 9-bromopropyl aminoacridine together with the 9-aminoacridine in the organic solvent, and recrystallizing to obtain the bridge-linked acridine dimer. The preparation method for the bridge-linked acridine dimer is simple, and mild in reaction conditions; the yield is relatively high; the bridge-linked acridine dimer has relatively high anti-tumor activity, so that a new research direction is provided for preparation of anti-tumor drugs.

The invention discloses a method for preparing 1,3-bis[(trihydroxy)methylamino]propane. The method comprises the following steps: adopting trihydroxymethyl aminomethane and 1,3-dibromopropane as the main reaction materials; reacting in an ethanol solution under reflux for a certain time; respectively subjecting to the acidification and the alkalization treatment to obtain a coarse target product; and re-crystallizing to obtain a pure product. The method has the advantages that the preparation condition and process are optimized; the yield is 30% to 80% in terms of the ratio of an actual yield to a theoretical yield, and the product purity is 90% to 99.5% and the melting point is 164 to 165 DEG C..

The invention provides a preparation method of quaternized halamine modified graphene oxide antibacterial nanoparticles, and belongs to the technical field of antibacterial material synthesis. The method comprises the following steps: firstly, modifying 5,5-dimethylhydantoin by using 1,3-dibromopropane to prepare 3-bromopropyl-5,5-dimethylhydantoin for later use; then, grating 4-vinylpyridine on graphene oxide in situ; and finally, grafting 3-bromopropyl-5, 5-dimethylhydantoin to the modified graphene oxide, and carrying out chlorination with sodium hypochlorite, so as to obtain the quaternized N-halamine modified graphene oxide antibacterial nanoparticles. The quaternized halamine modified graphene oxide antibacterial nano material disclosed by the invention has an excellent antibacterial effect and can be recycled through a sterilization-chlorination-sterilization process. Meanwhile, contact sterilization and release sterilization functions are realized.

The invention provides a method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine, which comprises the following steps of a) carrying out gas chromatography detection on a sample to be detected, and calculating the content of the residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine according to the detection result and an established standard curve. A chromatographic column for gas chromatography detection is a capillary chromatographic column DB-624UI, the temperature of a sample inlet is 210-230 DEG C, and a detector is an electron capture detector. Compared with the prior art, the detection method provided by the invention has the advantages that optimized chromatographic conditions are adopted, and the detection effect on 1, 2-dibromoethane and 1, 3-dibromopropane is good; the detection method is high in accuracy, good in sensitivity, precision and durability, and suitable for detection of residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine.

The invention discloses a preparation method and an application of ethyl 2-(4-hydroxyphenyl)thiazole-4-carboxylate derivatives. The preparation method comprises the following steps: reacting p-hydroxythiobenzamide with ethyl 3-bromopyruvate to synthesize an intermediate ethyl 2-(4-hydroxyphenyl)thiazole-4-carboxylate, respectively reacting the intermediate with 1,3-dibromopropane, 1,4-dibromobutane or 1,5-dibromopentate to synthesize ethyl 2-(4-(3-bromopropoxy)phenyl)thiazole-4-carboxylate, ethyl 2-(4-(4-bromobutoxy)phenyl)thiazole-4-carboxylate or ethyl 2-(4-((5-bromopentyl)oxy)phenyl)thiazole-4-carboxylate, and respectively reacting the ethyl 2-(4-(3-bromopropoxy)phenyl)thiazole-4-carboxylate, ethyl 2-(4-(4-bromobutoxy)phenyl)thiazole-4-carboxylate or ethyl 2-(4-((5-bromopentyl)oxy)phenyl)thiazole-4-carboxylate with an amine to generate the target products. The synthesis method has the advantages of simplicity, safety and small pollution, and the products have a strong inhibition effect on butyrylcholine esterase and/or acetylcholinesterase, and can be used for preparing anti-Alzheimer disease medicines.

The invention discloses a tetra-azido alkane and a preparation method thereof. A structural formula of the tetra-azido alkane is (N3CH2)2CH(CH2)3CH(CH2N3)2. The preparation method comprises the following steps of: under the protection of nitrogen, reacting diethyl malonate and 1,3-dibromopropane at a low temperature to obtain tetracthyl-1,1,5,5-pentanctetracarboxylate; under the protection of the nitrogen, carrying out ice bath at below 5 DEG C, and reacting the tetracthyl-1,1,5,5-pentanctetracarboxylate and a tetrahydroaluminate diethyl ether solution to obtain 2,6-dihydromethyl-1,7-heptandiol; carrying out the ice bath at below 5 DEG C, reacting paratoluensulfonyl chloride and a pyridine solution of the 2,6-dihydromethyl-1,7-heptandiol for 10h, and carrying out chloroform recrystallization to obtain 2,6-p-ditoluenosulfonate methyl-1,7-p-ditoluenosulfonate methyl heptaester; and adding an aqueous solution of sodium azide to a dimethylformamide solution of the 2,6-p-ditoluenosulfonate methyl-1,7-p-ditoluenosulfonate methyl heptaester to react for 15h at 80 DEG C to obtain a 2,6-biazido-1,7-di-azido heptane product.

The invention discloses a preparation method of [3-(dimethylamino)propyl]triphenylphosphonium bromide hydrobromide. The preparation method is characterized by comprising the following steps: (1) 180-220 kg of toluene is pumped into a reaction kettle, 80-100 kg of triphenyl phosphine is added manually, 50-70 kg of 1,3-dibromopropane is added dropwise at a relatively high speed to an elevated tank, flux is performed for 5-6 h at normal pressure and at the temperature of 80 DEG C, and P-I is obtained through cooling, filtering and drying; (2) 350-420 kg of methanol is pumped into the reaction kettle, 150 kg of P-I is added to methanol manually, 80-120 kg of a dimethylamine aqueous solution is added dropwise to the elevated tank, and a reaction is performed for 10-14 h at normal pressure and at the temperature of 50 DEG C after addition; (3) methanol is evaporated to dryness after the reaction, 360-450 kg of ethanol is pumped in, cooling, filtering and drying are performed after heating for dissolution, and [3-(dimethylamino)propyl]triphenylphosphonium bromide hydrobromide is obtained.

The invention relates to an intermediate and method used for preparing dronedarone and belongs to the technical field of cardiovascular drugs. The method comprises the following steps of: using 2-n-butyl-5-acetamidobenzobfuran to react with p-anisoyl chloride under the catalysis of Lewis acid and obtain 2-n-butyl-3-(4-methoxy-benzoyl)-5-acetamidobenzobfuran; acidizing to obtain 2-n-butyl-3-(4-methoxy-benzoyl)-5-benzofuranamin hydrochloride, reacting with methylsulfonyl chloride to obtain 2-n-butyl-3-(4-methoxy-benzoyl)-5-methylsulfonylamidobenzobfuran; obtaining 2-n-butyl-3-(4-hydroxyl-benzoyl)-5-methylsulfonylamidobenzobfuran under the action of the Lewis acid; and reacting with 1,3-dibromopropane to obtain 2-n-butyl-3-[4-(gamma-bromopropyl)hydroxyl-benzoyl]-5-methylsulfonylamidobenzobfuran, and then reacting with di-n-butylamine to obtain dronedarone. The method avoids the catalytic hydrogenation reaction and has the advantages of available raw materials, simple operation process, high yield, easiness in industrialization and the like.

The invention discloses a method of detecting the content of 1,1-dichloroacetone in drinking water by GC/MS combination. The method includes the following steps of: (1) adding a terminating agent ascorbic acid according to a ratio that 0.4-0.5 mmol of the terminating agent ascorbic acid is added for each liter of a drinking water sample; shaking uniformly, adjusting the pH value of the drinking water sample to be 4.0-6.0, adding anhydrous sodium sulfate according to a ratio that 6-8 g of the anhydrous sodium sulfate is added for each 25 mL of the mixture of the terminating agent ascorbic acid and the drinking water sample, oscillating until the salt is completely dissolved, and adding methyl tertiary butyl ether containing an internal standard substance 1,2-dibromopropane for extraction, with the volume ratio of the drinking water sample to the methyl tertiary butyl ether being 25:1-2; and (2) detecting the extract by using gas chromatography/mass spectrometer, performing quantitative detection by selecting an ion mode, and obtaining the content of the 1,1-dichloroacetone in the drinking water by adoption of an internal standard method. The method by the invention has advantages of rapidness and low cost.

The invention relates to a method for synthesizing NU-88 molecular sieves. The method comprises the following steps of (1) mixing 1,3-dibromopropane, 1-methyl-4-piperidone and a solvent, and carryingout a pre-reaction at 15-60 DEG C for 0.5-96 h to obtain a pre-reaction product, wherein a molar ratio of the 1,3-dibromopropane to the 1-methyl-4-piperidone to the solvent is 1 to (1.8 to 3) to (1 to20); and (2) mixing the pre-reaction product obtained in the step (1), an organic alkali, an inorganic alkali, an aluminium source, a silicon source and water to obtain a to-be-crystallized mixture,conducting hydrothermal crystallization treatment on the to-be-crystallized mixture, and recovering a solid product. According to the disclosed method, necessary tedious processes, including high-costseparation and purification, of conventional synthesis of a NU-88 molecular sieve template are omitted, large time consumption, energy consumption and material consumption are avoided, and the cost reduction effect is obvious.

The invention provides a solvent for removing underground heavy hydrocarbon deposition and a preparation method thereof. The preparation method comprises the following steps of coating the surfaces of Fe3O4 nanoparticles with polythiophene to obtain Fe3O4 nanoparticles coated with polythiophene, preparing a first solvent with a diamine structure by utilizing alkylation reaction between 1, 3-dibromopropane and diethylamine, reacting the first solvent with the Fe3O4 nanoparticles coated with polythiophene to obtain a second solvent, and finally, mixing the second solvent with oleic acid, 150# solvent oil and water according to a preset volume ratio to obtain the solvent for removing underground heavy hydrocarbon deposition. By means of the mode, the first solvent can be used for conducting amination modification on the nanoparticles, and the dissolving effect and viscosity reduction capacity of the solvent are effectively improved; and the second solvent is mixed with oleic acid, 150# solvent oil and water, so that the dissolving capacity and viscosity reduction effect of the solvent are further improved, the effect of removing underground heavy hydrocarbon deposition is achieved, and the requirements of practical application are met.

The invention provides synthesis of a Gemini type cationic asphalt emulsifier--1,3-{N-[3-dodecyloxy polyoxyethylene ether(9)-2-hydroxy]propyl dimethyl}propane from aliphatic polyoxyethylene ether AEO-9, epichlorohydrin, dimethylamine and 1,3-dibromopropane. The Gemini type cationic asphalt emulsifier is used for preparing emulsified asphalt. The test results of the emulsified asphalt show that the prepared emulsified asphalt can be stably stored for 5 days when the usage amount of the emulsifier is 2.5% of the total amount of the emulsified asphalt. The Gemini type cationic asphalt emulsifier provided by the invention can be extensively applied to adhesive bonding layers, fog sealing layers and solvent-free cold mixing, and is used for recycling of asphalt and stabilization of a asphalt pavement base.

The invention provides a preparation method of gemfibrozil. The preparation method is characterized by comprising the following steps: carrying out a salt-forming reaction between starting materials, namely 2,5-dimethylphenol and diethyl malonate, under the action of alkali; carrying out a nucleophilic substitution between the reaction product and 1,3-dibromopropane; hydrolyzing in an aqueous solution of alkali and carrying out a decarboxylation reaction to generate 5-(2,5-dimethylphenoxyl)pentanoic acid; and carrying out a methylation reaction between the reaction product and dimethyl sulphate (V) under the action of alkali so as to generate gemfibrozil. The preparation method has simple processing steps, reaction conditions are not harsh, synthesis route has no special requirements on equipment, investment cost of production equipment is greatly reduced, and it is easy to realize industrial production. The raw materials are easily available in the market, and cost is relatively low. Thus, industrial cost reduction is realized.

The invention provides a preparation method of high-strength composite hydrogel. The preparation method comprises the following steps: firstly, carrying out a coupling reaction on 1-vinyl imidazole and a monomer A (1, 2-dibromoethane, 1, 3-dibromopropane, 1, 4-dibromobutane and the like) to obtain a cross-linking agent A, then adding 3-[2-(methacryloyloxy) ethyl] trimethylammonium] propane-1-sulfonate (MPS), a monomer B (vinyl-containing imidazole bromide), the cross-linking agent A and a water-soluble photoinitiator into water, under the protection of N2, carrying out ultraviolet light induced polymerization reaction to establish covalent bond cross-linking and ionic interaction polyion liquid hydrogel, soaking the polyion liquid hydrogel by adopting a metal ion salt solution, and chelating metal ions with imidazole active sites in the soaking process to obtain the high-strength composite hydrogel. The hydrogel prepared by the method has excellent self-repairing property and mechanical property, is high in antibacterial property, and has potential application value in the aspects of bioengineering, metal catalysis and the like.