192 results about "Bromosuccinimide" patented technology

The invention provides a stilbene derivative with 1,3,4-oxadiazole and a preparation method and application thereof. The preparation method of the stilbene derivative with 1,3,4-oxadiazole comprises four specific reaction steps, namely oxidation cyclization reaction, NBS (N-bromosuccinimide) bromination reaction, triethyl phosphite esterification reaction and Wittig-Honner reaction. The stilbene derivative with 1,3,4-oxadiazole disclosed by the invention can be used to obviously inhibit the growing activities of Lepidopteron such as beet armyworm and cabbage looper and have important application value in the developments of environmentally friendly, efficient and new pesticides.

The invention discloses a preparation method of an ozagrel bulk drug. The method comprises the following steps of: bromating methyl ethyl cinnamate serving as a starting material with NBS (B-Bromosuccinimide) to obtain ethyl 4-bromomethylcinnamate; undergoing a condensation reaction on the ethyl 4-bromomethylcinnamate and imidazole to generate ozagrel ethyl ester; hydrolyzing under an alkaline condition; performing acid precipitation to obtain crude ozagrel; and refining to obtain an ozagrel bulk drug. Due to the adoption of the method, a method for refining catalysts, solvents and crude products used in each reaction step is improved, the product yield is high, the product quality is good, the use of toxic reagents and expensive reagents is avoided, little environmental pollution is caused, and the production cost is low. The method is suitable for industrial production, and is an improved and environmentally-friendly method for preparing the ozagrel bulk drug.

The invention relates to the field of olefin catalytic polymerization, and aims at providing a vinylene acenaphthene (alpha-diimine) nickel olefin catalyst, and preparation and an application thereof.The preparation comprises the typical synthetic steps: carrying out a diacylation reaction of acenaphthene to obtain a compound C1; carrying out a bromination reaction of the compound C1 and N-bromosuccinimide (NBS) to obtain a compound C2; carrying out an elimination reaction of the compound C2 to obtain a compound C3; carrying out ketone amine condensation reaction of the compound C3 with symmetric aniline, to obtain alpha-diimine ligands C4-C8; and under anhydrous and anaerobic conditions, complexing the alpha-diimine ligands C4-C8 with ethylene glycol dimethyl ether nickel dibromide to obtain a final product. The catalyst has higher activity and better thermal stability, and can catalyze ethylene with high activity at the temperature of greater than or equal to 60 DEG C to obtain high-molecular-weight hyperbranched polyethylene. Under the same polymerization conditions, ethylene can be catalyzed to polymerize to obtain branched polyethylene with higher molecular weight, so as to meet more application requirements. The cost of raw materials is low, the reaction yield is high and industrialized production can be achieved.

The invention discloses an aggregation-induced emission near-infrared emission diketopyrrolopyrrole compound and a preparation method thereof. The method comprises the steps that 3,6-dithiophene diketopyrrolopyrrole reacts with twice molar weight of alkyl bromide so as to obtain 2,5-dialkyl-3,6-dithienopyrrolopyrrole, then the 2,5-dialkyl-3,6-dithienopyrrolopyrrole sequentially undergoes Vilsmeierreaction with phosphorus oxychloride/N,N-dimethylformamide and undergoes substitution reaction with N-bromosuccinimide so as to obtain 2,5-dialkyl-3-(5-formyl)thienyl-6-(5-bromine)thienyl diketopyrrolopyrrole, and then the 2,5-dialkyl-3-(5-formyl)thienyl-6-(5-bromine)thienyl diketopyrrolopyrrole undergoes Suzuki reaction with tetraphenyl ethylene boric acid ester so as to obtain 2,5-dialkyl-3(4-((E)-2-phenyl-1,2-disubstituted styryl)phenyl)thienyl-6-(5-formyl)thienyl diketopyrrolopyrrole. The compound has the emission range greater than 650 nm and has the aggregation-induced emission property.

The invention discloses a preparation method of phloroglucinol, which comprises the following steps: dissolving resorcinol in reaction solvent, then adding an N-bromosuccinimide solution, heating to perform bromination reaction, and then treating to obtain 4-bromoresorcinol; adding the obtained 4-bromoresorcinol into a container, adding reaction solvent, strong alkali and a catalyst, heating to perform hydrolysis reaction, and then treating to obtain a phloroglucinol salt solution; and adding hydrochloric acid into the phloroglucinol salt solution to regulate the pH value and precipitate solid, filtering to obtain the solid phloroglucinol crude product, and finally purifying to obtain the phloroglucinol product. According to the preparation method, the low-price accessible resorcinol is used as the raw material and is subjected to bromination, strong alkali hydrolysis and acidification, thus preparing the phloroglucinol. According to the invention, the reaction time is shortened, the production cost is lowered, and remarkable economic benefits are achieved. By preparing the phloroglucinol through the preparation method, the yield is up to 70% or above, and the purity of the prepared product is up to 99.9% or above.

The invention discloses an o-carborane derivative and a synthesis method thereof. The method includes: step 1, taking 5-fluoro-2-methyl-1H-indene or 5-trifluoromethyl-2-methyl-1H-indene as a reactioninitiator, adopting aluminum trichloride as a catalyst, and carrying out reaction with 1-chloroacetic acid to obtain an intermediate 2; step 2, reacting the intermediate 2 with N-bromosuccinimide by taking DMF as a reaction solvent to obtain an intermediate 3; and step 3, reacting the intermediate 3 with o-carborane in an organic solvent or ionic liquid under an alkaline condition to obtain the corresponding o-carborane derivative. According to the invention, fluorine ions and relative hydrophilic groups are introduced for modification through chemical synthesis, the purposes of reducing toxicity and increasing compound polarity and cell affinity are achieved, so that the technical effect of targeted enrichment and high concentration of boron ions in tumor cells is achieved, and then the technical bottleneck that p-borane phenylalanine (BPA) is discharged by an "anti-transport" mechanism after the concentration of the BPA in the tumor cells reaches a certain number 1 is solved.

The invention discloses a method for synthesizing 5-isoindolone chloride, comprising the following steps: using 4-chlor-2-methyl benzoic acid as an initial reactant; obtaining products through methylation, NBS (N-bromosuccinimide) bromination reaction and amidation reaction in sequence; and obtaining a monobromo pure product through firstly double bromination and then debromination in the NBS bromination reaction. According to the method for synthesizing, the doping of double brominated products when NBS is excessive in the prior art is overcome, and processing is ensured after raw materials are completely reacted without detecting and tracking reaction under the condition that NBS is excessive, so that the cost is reduced, the reaction is easy to control, the complexity of operation is reduced, the purification is relatively simple, and the 5-isoindolone chloride is easy to produce in large scale.

The invention provides a metal organic framework based on imidazole sulfonic acid as well as a preparation method and application. The metal organic framework based on the imidazole sulfonic acid is obtained by synthesizing and modifying a metal organic framework based on an imidazole ligand through a sulfonic compound; a chemical structural formula of the metal organic framework based on the imidazole ligand is [Zr6O4(OH)4L6]n, wherein n is a natural number more than 0; L is an organic ligand L and a chemical structural formula of the organic ligand L is show in the description; a synthesis method of the organic ligand L comprises the following steps: firstly, enabling 3-methyl-terephthalic acid to react to obtain an intermediate A; secondly, taking the intermediate A and bromosuccinimide as raw materials and reacting to obtain an intermediate B; thirdly, taking the intermediate B and imidazole as raw materials and reacting to obtain an intermediate C; finally, carrying out hydrolysis reaction on the intermediate C to prepare the organic ligand L. The metal organic framework based on the imidazole sulfonic acid has a catalytic effect on benzaldehyde under normal pressure and has the characteristics of moderate reaction conditions, short reaction time, less dosage of a catalyst and capability of being recycled and repeatedly utilized.

The invention relates to reductive cation polymethacrylate, a preparation method thereof, application of the polymethacrylate to establishment of gene nano-complexes and application of the polymethacrylate to gene therapy. The method comprises the following steps: 1, 3, 5-triisopropylphenyl is taken as a raw material and reacts with N- bromosuccinimide and potassium ethyl xanthate to obtain substituted 1, 3, 5- triisopropylphenyl potassium ethyl xanthate; and the substituted 1, 3, 5- triisopropylphenyl potassium ethyl xanthate is catalyzed by azo-bis-iso-butyrynitrile, and subjected to reversible addition-broken strand transfer polymerization, aminolysis and oxidation reaction with 2-(dimethylamino ethyl)metacrylic acid ester to obtain poly (1, 3, 5-three-terminal sulfhydryl (2-propyl phenyl -2-(dimethylamino)ethyl)) methacrylic acid ester) and disulfide bond crosslinking products of the poly (1, 3, 5-three-terminal sulfhydryl (2-propyl phenyl -2-(dimethylamino)ethyl)) methacrylic acid ester). The polymethacrylate can condense plasmid genes into nano complexes; the transfection efficiency of HEK293T cells and Hella cells is more than 30 percent; the toxicity is low; and the survival rate of the cells is more than 80 percent.

The invention discloses a supported platinum complex oxidizing agent easy to recycle. The supported platinum complex oxidizing agent is provided with the structure shown in the formula I. The invention further provides a preparation method of the oxidizing agent. The method comprises the steps that 1, pyridine is taken as solvent, and polystyrene microsphere is reacted with toluene sulfonyl chloride to obtain a yellow solid substance; 2, ultrasonic dispersion is conducted on the obtained yellow solid substance in ethylenediamine, and the yellow solid substance is subjected to stirring reactionto obtain a deep yellow solid substance; 3, DMF is taken as solvent, and the obtained deep yellow solid substance and a two-valence platinum complex are subjected to stirring reaction to obtain a black solid substance; 4, after ultrasonic dispersion is conducted on the black solid substance in ethyl alcohol, the black solid substance is fully reacted with N,N'-bromosuccinimide to obtain a light black solid substance, namely the supported platinum complex oxidizing agent. The oxidizing agent preparation method is simple, recycle is easy, and the reaction yield is high.

The invention relates to a preparation method for a medicine KCNQ potassium channel conditioning agent critical material 2-bromine-4,6-dichloroaniline. According to the invention, 2,4-dichloroaniline is taken as a raw materials, and is subjected to NBS (N-bromosuccinimide) bromination to obtain a target object, and the preparation method of the invention has the advantages of low preparation method and simple operation, and has industrial production value.

The invention discloses a preparation method of 2, 3-thiophenedicarboxaldehyde and belongs to the field of organic synthesis. The preparation method is characterized in that 2, 3-thiophenedicarboxaldehyde as a raw material and N-bromosuccinimide undergo a bromination reaction in the presence of benzoyl peroxide as a catalyst and carbon tetrachloride or trichloromethane as a solvent at a certain temperature to produce 2, 3-di(bromomethyl)thiophene; and 2, 3-di(bromomethyl)thiophene and hexamethylenetetramine undergo a Sommelet reaction in the presence of trichloromethane as a solvent at a certain temperature to produce 2, 3-thiophenedicarboxaldehyde. Compared with the prior art, the preparation method has the advantages that raw materials are cheap and easily available; reaction conditions are mild and can be controlled easily; and a product yield is high.

The invention relates to the field of organic synthesis, in particular to a method for preparing 2-bromo-fluorobenzyl bromide, which comprises the following steps: (1) in the presence of an organic or inorganic solvent, adding a 2-bromo-6-fluorotoluene compound and 40-mass-percent hydrobromic acid and dripping 30-mass-percent hydrogen peroxide under a lighting condition, and reacting for 6 to 24 hours, wherein the molar ratio of 2-bromo-6-fluorotoluene to HBr is 1:(1-3.5) and the molar ratio of the 2-bromo-6-fluorotoluene to H2O2 is 1:(1-3.5); and (2) washing the reaction solution with saturated sodium sulfite solution and water, drying the reaction solution with anhydrous sodium sulfate, evaporating solvent under a reduced pressure, and obtaining the 2-bromo-6-fluorotoluene compound by silica gel column chromatography. In the method, the hydrobromic acid and hydrogen peroxide are used in place of the traditional N-bromosuccinimide brominating agent, so the production cost is reduced; and lighting is used in place of a benzoyl peroxide initiator, so method has the advantages of mild reaction conditions, high product purity, high yield and the like.

The present invention provides a p-bromomethyl phenylacetic acid preparation method, which comprises: dissolving p-methyl phenylacetic acid in a high boiling point solvent, wherein the solvent is benzene, chlorobenzene or dichlorobenzene; adding a brominating agent and a catalyst, wherein the brominating agent is bromine or bromosuccinimide, the catalyst is azobisisobutyronitrile or benzoyl peroxide, and a molar ratio of the p-methyl phenylacetic acid to the brominating agent is 1:0.8-2.0; heating to a temperature of 80-130 DEG C, carrying out a reaction for 6-12 h through the initiation with incandescent light irradiation, and cooling; and filtering, and carrying out water washing to obtain the p-bromomethyl phenylacetic acid. According to the present invention, the high boiling point reaction solvent is used, a lot of the generated heat can be taken away by the high boiling point solvent through the circulation after the reaction is initiated by the illumination, the product p-bromomethyl phenylacetic acid is precipitated from the solvent after the cooling, and the water washing and the drying are performed to obtain the product, wherein the HPLC purity of the product is greater than 98.5%, and the yield is up to 90%.

The invention discloses a cyclopenta(2,1-b:3,4-b')dithiophene-thieno[3,4-b]pyrazine conjugated polymer of a general formula (I) and a preparation method and use thereof. The preparation method comprises: reacting a diketone compound with 3,4-diaminothiophene.hydrogen chloride; subjecting the product of the reaction to bromination with N-bromosuccinimide (NBS) to obtain a target monomer; and underan oxygen-free condition, subjecting the 4,4-dialkyl-2,6-bis(trimethylstannyl)-cyclopenta(2,1-b:3,4-b')dithiophene, 4,4-dialkyl-2,6-dibromo-cyclopenta(2,1-b:3,4-b')dithiophene and the target monomer to polymerization to obtain the product disclosed by the invention. The preparation method disclosed by the invention is simple, makes operation and control easy, and is suitable for industrial production. Because a long-chain alkyl is introduced into the molecule of the polymer, the solubility and processability of the polymer are improved. The polymer can be widely used in fields of polymer solar cells and the like.

The invention relates to the field of olefin catalytic polymerization, and aims to provide an improved (alpha-diimine) nickel catalyst as well as a preparation method and application thereof. The chemical structural formula of the (alpha-diimine) nickel olefin catalyst is shown as a formula (II), in the formula, R1 is alkyl, and R2 is halogen. The preparation method of the catalyst Cat-B comprises the following steps: carrying out diacylation reaction on acenaphthene to obtain a compound C1; subjecting the C1 and N-bromosuccinimide to a bromination reaction to obtain C2; carrying out elimination reaction on the C2 to obtain C3; subjecting the C3 and symmetrical aniline to a ketoamine condensation reaction so as to obtain the alpha-diimine ligand C4; and carrying out complexing on the C4 and ethylene glycol dimethyl ether nickel dibromide to obtain the catalyst Cat-B. Compared with existing catalysts, the branched polyethylene obtained by catalyzing ethylene polymerization under the same condition can be simultaneously improved in terms of branching degree and molecular weight, the comprehensive performance of the branched polyethylene in the aspects of strength and elasticity can be improved, and the application scene of the branched polyethylene in the aspect of rubber products is expanded.

The invention discloses a method for synthesizing beta-brominated alcohol by an anisotropic emulsion microreactor. Anisotropic emulsion liquid drops are used as a micro-reactor, reaction raw materials, namely olefin and N-bromosuccinimide (NBS), are selectively dissolved in an n-heptane phase and a surfactant aqueous solution phase which are mutually insoluble respectively, fluorocarbon oil is selected as a third phase, an anisotropic emulsion with fluorocarbon oil/n-heptane as an internal phase and a surfactant aqueous solution as an external phase is prepared by a one-step vortex oscillation method; two reaction raw materials are selectively solubilized and isolated by a multi-phase microcell of anisotropic emulsion droplets, meanwhile, the characteristics of multi-phase interfaces and multi-microstructures of the anisotropic droplets are fully exerted, so that static controllable synthesis of beta-brominated alcohol is realized without continuous stirring. The method has the advantages of simplicity and convenience in operation, low energy consumption, controllable reaction rate and easiness in product recovery.

The invention discloses a preparation method of a high-performance carboxyl-terminated low-molecular-weight fluorine-containing polymer, belonging to a polymer preparation method. According to the invention, a carboxyl-terminated low-molecular-weight fluorine-containing polymer containing double bonds in a chain and prepared by an oxidative degradation method is used as a raw material, a fluorinated addition reaction system and method for the fluorine-containing polymer are created, N-fluoro-N'-(chloromethyl)triethylenediamine bis(tetrafluoroborate) or a hydrogen fluoride complex and the likeare used as fluorinating reagents, lithium aluminum hydride or borohydride is used as a hydrogenation reagent, silver fluoride and the like are used as nucleophilic reagents, and N-bromosuccinimide and the like are used as electrophilic reagents, so a fluorine content is increased while saturation of double bonds in a chain is realized, and the thermal stability of the polymer is greatly improved.The method is simple in process, mild in reaction conditions and high in efficiency; a saturation rate reaches 80% or above, the fluorine content of the produced polymer is higher than 66%, and the polymer can serve as a fluorine-containing precursor of a functional polymer and an additive manufacturing (3D printing) raw material and can also be applied as a high-performance adhesive, a joint mixture, a coating, a processing compounding agent and the like.

The invention relates to a tricyclic thiazolo[5,4-d]pyrimidone derivative and application thereof. The derivative is prepared by the steps that ethyl cyanoacetate serves as an initial raw material, a hydroxylamine compound (A) is generated under the action of sodium nitrite and phosphoric acid, ethyl 2-aminocyanoacetate (B) is obtained through reduction of sodium hydrosulfite and reacts with acetic anhydride and a Lawesson's reagent separately to obtain5-amino-4-formate thiazole compounds (D), NBS (N-bromosuccinimide) bromination is conducted, a 2-bromo-dihydropyrrolo[1,2-a]thiazolo[5,4-d]pyrimidinone compound (F) and a 2-bromo-7,8-dihydro-5H-pyridino[1,2-a]thiazolo[5,4-d]pyrimidin-10(6H)-one derivative (G) are obtained under the action of phosphorus oxychloride, and finally Suzuki coupling reaction is conducted to obtain 64 differently-substituted tricyclic thiazolo[5,4-d]pyrimidone derivatives H1-H32 and I1-I32. The inhibitory activity of the 64 compounds on acetylcholinesterase/butyrylcholinesterase in Alzheimer's disease and the antibacterial activity of Candida albicans, and the result shows that 46 compounds have strong inhibitory activity on acetylcholinesterase/butyrylcholinesterase, and 27 compounds have inhibitory activity on candida albicans.