20 results about "Phthalimide" patented technology

The invention discloses four-arm polyethylene glycol amine as well as a preparation method and application thereof, relates to the technical field of high polymer materials, and solves the problems of poor comprehensive properties such as strength, fatigue resistance and swelling resistance when traditional dual-network hydrogel is applied to preparation of a cartilage repair material in the prior art. The molecular weight of four-arm polyethylene glycol amine provided by the invention is 10 kDa or 40 kDa, four-arm polyethylene glycol, phthalimide, diisopropyl azodicarboxylate and triphenylphosphine are subjected to a Mitsunobu reaction and hydrazinolysis, and the four-arm polyethylene glycol amine with the molecular weight of 10 kDa is obtained; four-arm polyethylene glycol, phthalimide, diisopropyl azodicarboxylate and triphenylphosphine are subjected to a Mitsunobu reaction and hydrazinolysis, and four-arm polyethylene glycol amine with the molecular weight of 40 kDa is obtained. The double-network hydrogel prepared from the four-arm polyethylene glycol amine has excellent comprehensive performance such as high mechanical strength, fatigue resistance, self-recovery performance and swelling resistance, and can be applied to preparation of cartilage-like materials.

The application provides a preparation method of a rare earth metal adsorption and separation resin and a resin extraction column. The preparation method comprises the following steps: adding an oil phase composed of styrene, divinylbenzene, a pore former and an initiator into an aqueous phase containing a dispersant and an inorganic salt to perform suspension polymerization, so as to obtain a white ball resin; performing phthalimide and hydrolysis on the white ball resin, so as to obtain a primary amine resin; performing reaction on the primary amine resin with chloroacetic acid and an alkaline medium, so as to perform carboxymethylation on part of the primary amine sites; and performing reaction on the obtained intermediate resin with phosphorous acid, formaldehyde and an acidic medium, so as to perform phosphonic acid methylation on the remaining part of the primary amine sites. The white ball resin is first subjected to amination, and then part of the carboxymethylation and part of the phosphonic acid methylation are sequentially performed, so that the carboxyl type chelation sites and the phosphonic acid type chelation sites are simultaneously reserved in the same resin bead, thereby being beneficial to improving the comprehensive adsorption performance and separation performance of the resin on the rare earth metal.

Four-arm polyethylene glycol amine and preparation method and application thereof, relate to the technical field of high polymer materials, and solve the problem of poor comprehensive performance such as strength, fatigue resistance and swelling resistance when the traditional double network hydrogel is applied to the preparation of cartilage repair materials in the prior art. The four-arm polyethylene glycol amine provided by the application has a molecular weight of 10 kDa or 40 kDa. Four-arm polyethylene glycol, phthalimide, diisopropyl azodicarboxylate and triphenylphosphine are subjected to Mitsunobu reaction and hydrazinolysis to obtain four-arm polyethylene glycol amine with a molecular weight of 10 kDa. Four-arm polyethylene glycol, phthalimide, diisopropyl azodicarboxylate and triphenylphosphine are subjected to Mitsunobu reaction and hydrazinolysis to obtain four-arm polyethylene glycol amine with a molecular weight of 40 kDa. The double network hydrogel prepared from the four-arm polyethylene glycol amine has excellent comprehensive performance such as high mechanical strength, fatigue resistance, self-recovery and swelling resistance, and can be applied to the preparation of cartilage-like materials.

The application discloses a synthesis method of C3-substituted quinoxaline ketone derivatives and application thereof. A series of C3-substituted quinoxaline ketone derivatives with both terpene and quinoxaline ketone biological activity skeletons are obtained by using N-alkoxy phthalimide and quinoxaline ketone as starting substrates, under the catalysis of a photocatalyst and visible light irradiation, and at a temperature of 55-65 DEG C for 10-15 h. The application has the advantages of stable and easy-to-prepare raw materials, mild reaction conditions, simple experimental operation, good chemical selectivity and functional group tolerance, and is a green chemical synthesis method with good application prospect. The activity experiment results show that the synthesized C3-substituted quinoxaline ketone derivatives have good inhibiting effect on the growth of plant pathogenic fungi.

The application discloses a production process of trans-zeatin, which comprises the following steps: refluxing E-2-(4-hydroxy-3-methyl-2-butene)-phthalimide with sodium hydroxide in methanol to obtain (E)-4-amino-1-hydroxy-2-methyl-2-butene; filtering and collecting the filtrate and concentrating the filtrate; and reacting the concentrated filtrate with 6-chloropurine in n-propanol and triethylamine as an acid-binding agent to finally obtain trans-zeatin. The application uses E-2-(4-hydroxy-3-methyl-2-butene)-phthalimide as a raw material, and high-purity trans-zeatin is obtained through two steps. The preparation method can effectively improve the yield of trans-zeatin, is simple and convenient to operate, is convenient for industrial popularization, and has good economic and social benefits.

The invention relates to the field of isopropyl alcohol preparation, and discloses a chelate resin and a preparation method thereof, and a method for preparing electronic grade isopropyl alcohol, the method comprises the following steps: styrene-divinylbenzene polymeric microspheres are contacted with N-hydroxymethyl phthalimide, and an imidization reaction, a hydrolysis reaction and a carboxylation reaction are sequentially carried out. By using the chelate resin and the method for preparing the electronic-grade isopropanol, the content of isopropanol in the product can be effectively increased, and the content of water, zwitterions and particles can be reduced.

The invention relates to a preparation method of 3-bromo-2-methyl-6-methylsulfonyl benzaldoxime, and belongs to the technical field of pesticides. The preparation method comprises the following steps: by taking 2, 3-dimethyl-4-methylsulfonyl bromobenzene as a raw material and adopting an organic solvent, adding a metal salt catalyst and N-hydroxyphthalimide, dropwise adding n-butyl nitrite into a system at a certain temperature, carrying out a heat preservation reaction after dropwise adding, and carrying out post-treatment after the reaction is finished, so as to obtain the 3-bromo-2-methyl-6-methylsulfonyl benzaldoxime. According to the invention, the dosage of the oximation reagent n-butyl nitrite is reduced, and the yield of oximation reaction is improved. According to the method, the reaction conditions are mild, low-temperature dropwise adding and high-temperature reaction are converted into normal-temperature reaction, meanwhile, the reaction time is shortened, and the production energy consumption is reduced.

The application discloses a preparation method of functionalized polyolefin and belongs to the technical field of polymer modification. The preparation method comprises the following preparation steps: uniformly mixing polyolefin, grafting monomers and high-valence iodine compounds, and then heating and reacting to obtain the functionalized polyolefin; wherein the grafting monomers are at least one selected from N-hydroxy phthalimide and derivatives thereof and N-hydroxy succinimide and derivatives thereof. The preparation method uses high-valence iodine compounds as initiators, can preferentially activate polyolefin molecular chains, and forms a pre-combination body with the grafting monomers, thereby greatly inhibiting the non-selective initiation of beta-scission degradation and inter-chain crosslinking of free radicals on the polyolefin main chain, maintaining the stability of the base molecular weight, and realizing efficient grafting of the grafting monomers.

The application discloses a kind of synthesis methods of high-purity 2-bromo-6-nitrobenzaldehyde, belong to organic synthesis technical field, the synthesis method is at 20-30 ℃, 1,2-dichloroethane, 2-bromo-6-nitrotoluene is mixed, stirring is dissolved, N-bromine phthalimide and initiator are mixed, heating to 70-100 ℃, reflux reaction, cooling to 20-30 ℃, post-processing is obtained compound A;Compound A is mixed with acetonitrile, temperature control is 0-10 ℃, batch is added urotropine, stirring is at 20-40 ℃, acetic acid is added, stirring is at 70-100 ℃, post-processing is obtained 2-bromo-6-nitrobenzaldehyde;The synthesis method of the application can solve the problems of low product yield, low purity, poor quality, serious three waste pollution, high cost and difficult industrialization existing in the prior art of 2-bromo-6-nitrobenzaldehyde synthesis method.

This invention discloses a method for preparing 1,2,3,6-tetrahydrophthalimide, comprising the following steps: using cis-1,2,3,6-tetrahydrophthalic anhydride as the reaction substrate and a gradient-release composite ammonia source as the ammonia donor, a cyclization reaction is carried out in an ionic liquid reaction system to obtain a crude reaction solution containing 1,2,3,6-tetrahydrophthalimide; the obtained crude reaction solution is cooled to crystallize, solid-liquid separation is performed, and drying is carried out to obtain 1,2,3,6-tetrahydrophthalimide; the ionic liquid reaction system uses an imidazole-based ionic liquid as the main reaction medium; the gradient-release composite ammonia source is composed of a first ammonia source and ammonium acetate; the preparation method provided by this invention, through the buffering effect of the gradient-release composite ammonia source combined with the imidazole-based ionic liquid, combined with a segmented temperature-controlled reaction scheme, matches the ammonia consumption requirements at different stages of the cyclization reaction, effectively suppresses the carbon-carbon double bond polymerization side reaction, reduces impurity generation, and significantly improves the yield and purity of the product.

This invention belongs to the field of chemical intermediate preparation technology, and particularly relates to a method for recovering N-hydroxymethyl phthalimide from the residue of a key intermediate of 4-AA. The method includes the following steps: (1) Distillation: The toluene mother liquor produced from the preparation of methyl 2-(N-phthaliminomethyl)-3-oxobutyrate, a key intermediate of 4-AA, is filtered and distilled to obtain toluene solvent and concentrated residue. The toluene solvent is recovered and reused. (2) Hydrolysis: A hydrolysis reagent is added to the concentrated residue, with a weight ratio of concentrated residue to hydrolysis reagent of 1:(1.1-4). The mixture is heated to 30-100℃ and kept at this temperature for 1-10 hours with stirring to obtain a hydrolysis product. (3) Recovery: The hydrolysis product is cooled, crystallized, filtered, and washed with water to obtain N-hydroxymethyl phthalimide. This invention can recover effective components from hazardous waste, thereby reducing the discharge of hazardous waste and lowering the cost of hazardous waste treatment.

The present application relates to the fields of medicine, organic chemical industry and fine chemical industry, and particularly relates to an alkyl trifluoromethyl sulfide compound and a synthesis method thereof. Under the protection of inert gas, a non-activated alkene is used as a substrate, N-trifluoromethyl thiosaccharin or N-trifluoromethylthio phthalimide is used as a trifluoromethylthio source, cyclohexyl mercaptan, p-methyl phenyl mercaptan or 2-methyl mercaptoacetate is used as a hydrogen source, inorganic alkali and organic photocatalyst are added in a reaction system, blue light is irradiated, and different substituted alkyl trifluoromethyl sulfide compounds are synthesized under room temperature conditions. The trifluoromethylthio reagent used in the present application is easy to prepare and has good stability, and the participation of noble metal silver salt is avoided. A 7.5% sodium hypochlorite solution is used for post-treatment to remove the unreacted mercaptan. The synthesis reaction condition involved in the present application is mild, the reaction efficiency is high, the regioselectivity is good, the universality is excellent, and the functional group compatibility is good.

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing 4-acetylpyridine from pyridine, which comprises the following steps: reacting pyridine serving as an initial raw material with acetic anhydride and iron powder to obtain an intermediate 4-ethylpyridine; and carrying out catalytic oxidation to obtain the target product 4-acetylpyridine. According to the method for preparing 4-acetylpyridine, the reaction steps are few, the raw material price is low, and the catalyst used in the oxidation reaction can be recycled, when 4-ethylpyridine is synthesized, after iron powder is added, the problems that in the heat preservation reaction stage, the fluidity of reaction liquid becomes poor, and a stirring paddle is locked are solved by adopting a xylene adding mode; water is removed before rectification, so that the problem of ternary azeotropy of water, pyridine and 4-ethylpyridine is solved; before the oxidation reaction, the conversion rate is obviously improved by vacuumizing oxygen replacement and adopting a micro-positive pressure reaction mode, and the catalyst N-hydroxyphthalimide can be recycled, so that the method has a relatively good application value.

The application provides a synthesis method of a GLP-1 receptor agonist core chiral intermediate, which comprises the following steps: synthesizing a three-membered ring under alkaline conditions by using commercially available benzhydrylideneaminoacetonitrile or N-acetonitrile phthalimide and a compound shown in formula II which is a commercially available chiral pure intermediate; separating and purifying by recrystallization; removing a benzophenone protecting group under acidic conditions or removing a phthaloyl protecting group under a hydrazine hydrolysis condition; and forming a hydrochloride salt to obtain a target product. The application provides a relatively economical and environment-friendly synthesis technical route which is beneficial to scale-up production. The starting material of the application has a simple structure and is easily purchased in a commercial batch.

The invention relates to a continuous production method of scorch retarder CTP intermediate phthalimide, which comprises the following steps: taking phthalic anhydride and urea as raw materials, carrying out vacuum suction and mixing under the protection of nitrogen, and then feeding into a sectional screw conveyor for reaction. The inside of the screw conveyor is divided into four stages, namely a pretreatment stage, an imidization stage, a main reaction stage and a heat preservation reaction stage through partition plates, and the temperatures of the stages are controlled at 80 DEG C, 120 DEG C, 145-160 DEG C and 160 DEG C respectively. By arranging a first collecting port, a second collecting port and three groups of conveying channels, gas in the pretreatment stage is recycled as conveying power, and gas in the main reaction stage is recycled after impurity removal and pressurization. Through four-section temperature control, directional gas control and resource recycling, the problems of equipment corrosion, low raw material utilization rate, high energy consumption, unstable product purity and the like are effectively solved, and efficient, stable and continuous production of phthalimide is realized.

The application relates to the technical field of gas dust removal, in particular to a dust removal and filtration device for drying phthalimide, which comprises a dust removal box body, a conveying port is formed in one side of the dust removal box body, a reflux pipe is fixedly installed in the conveying port, a heat exchange box is fixedly installed at the other end of the reflux pipe, and a heat exchange assembly is fixedly installed in the heat exchange box; dust gas enters multiple heat exchange pipes through a gas shunt shell, contacts heat exchange water in the heat exchange box when entering the heat exchange pipes, the dust gas is cooled at the same time, the temperature of the water body is increased, the filtered purified water filters particulate matters in the interior through a liquid exchange filter plate, and the water body is re-entered into the heat exchange box for heat exchange through the circulation of a water pump, high-temperature dust gas is pretreated and cooled, the problem that the dust removal efficiency is seriously reduced due to the instantaneous gasification of the high-temperature dust gas when the high-temperature dust gas contacts water mist with excessively high temperature is prevented.

The application discloses an organic amine small-molecule catalyst with a chiral ure structure, a preparation method and application, and belongs to the technical field of organic amine compound preparation. The preparation method uses an o-phenylenediamine compound as a starting material, and sequentially performs steps of selective amino protection, ure bond construction, removal of an amino protecting group and reductive amination, so that the target catalyst can be efficiently constructed with good yield. The catalyst is applied to a kinetic ester exchange resolution reaction of a carboxylic acid phthalimide ester, can effectively resolve chiral substrates, and provides an efficient candidate approach for new drug creation.

The present application relates to the technical field of rubber material, in particular to a kind of high-temperature-resistant rubber material for LED light source packaging and preparation method thereof, for solving the problem that the physical performance of existing LED packaging material will deteriorate under high temperature environment, thereby affecting the stable operation of LED;The rubber material is added with sulfur fluorene type bisfluorene phthalimide-benzimidazole modified polyimide, first synthesized sulfur fluorene type bisfluorene phthalimide containing carboxyl, and then synthesized sulfur fluorene type bisfluorene phthalimide-benzimidazole containing nitro by using carboxyl and 4-nitro-o-phenylenediamine, the nitro is reduced to amino, and the intermediate product 5 containing amino is polymerized with 4,4'- (hexafluoroisopropyl) di-phthalic anhydride to form sulfur fluorene type bisfluorene phthalimide-benzimidazole modified polyimide, the heat resistance of the polymer is improved by sulfur fluorene type bisfluorene phthalimide structure and benzimidazole, and the working stability and service life of LED packaging under high temperature condition are effectively improved.

The application belongs to the technical field of molecular sieve catalysis and fuel cleaning, and particularly relates to a CoO x @Ti-SPP catalyst and a preparation method and application thereof. The CoO x @Ti-SPP catalyst is prepared by using Ti containing self-pillared pentasil (Ti-SPP) with a nanosheet self-supporting structure and a four-coordinated titanium site as a carrier, and loading CoO x active species. The CoO x active species can be highly dispersed on the surface of the Ti-SPP carrier and in-situ form stable Co-Ti synergistic active centers with the framework Ti sites, so that the molecular oxygen activation capacity of the catalyst is greatly improved. The CoO x @Ti-SPP catalyst exhibits excellent catalytic oxidation desulfurization activity on high steric hindrance and difficult to degrade thiophene sulfides in a reaction system taking air as an oxidant and trace N-hydroxy phthalimide or tert-butyl hydroperoxide as an initiator, and simultaneously has good cycle stability and recyclability.

A novel liquid comprising a mercapto-based compound, or hydrophobic sulfenyl chloride compound, such as perchloromethyl mercaptan (PCMM) and pentachloro ethyl mercaptan (PCEM), in the form of dispersed droplets having a size between 10 nanometers (~0.01µm) and 50 microns (50µm), wherein the liquid is a multiphasic system, exemplified by an oil in water emulsion where the droplets comprising the mercapto-based compound are dispersed as a discontinuous phase in water or an aqueous medium, being a continuous phase, and improved synthetic preparations of Phthalimide fungicidal compounds using the novel liquid as a reactant to enhance the process efficiency and quality of the synthesized Phthalimide obtained.