61 results about "Succinchlorimide" patented technology

The invention relates to a method for synthesizing an iodo-pyridine compound from N-propargyl enaminone, which comprises the following steps: by taking N-propargyl enaminone as a raw material, DMF (Dimethyl Formamide) as a reaction solvent and copper acetate and N-iodosuccinimide as accelerators, carrying out intramolecular coupling reaction at 60 DEG C to synthesize the iodo-pyridine compound. The method for directly synthesizing the pyridine heterocyclic compound through the intramolecular coupling reaction of the N-propargyl enaminone under the non-alkaline condition is disclosed for the first time, reaction substrates are not limited to benzene rings on alkynyl, the application range of the reaction is greatly expanded, and the method has the advantages of being wide in substrate range, strong in functional group application range, mild in reaction condition, easy to operate, safe, high in yield and the like. And raw materials are cheap.

This invention belongs to the field of coolant technology, specifically relating to a coolant and its application in an immersion liquid-cooled energy storage system. The coolant, by weight, comprises 80-95 parts base oil, 1-5 parts thermally conductive nanoparticles, 0.5-2 parts composite dispersant, 0.3-1 part composite corrosion inhibitor, 0.1-0.5 parts antioxidant, 0.2-0.5 parts pour point depressant, and 0.01-0.05 parts defoamer. The base oil is a mixture of polyalphaolefin and synthetic ester, and the composite dispersant is a compound of polyisobutylene succinimide and Mannich base dispersant. Aging tests show that this coolant exhibits high thermal conductivity retention, low acid value increase, and low corrosion rate. The coolant of this invention can effectively maintain the dispersion stability of nanoparticles in the environment of precipitates from sealing materials, extending the fluid change cycle.

The application belongs to the technical field of biological medicine, and discloses a synthesis method of aryl F-18 labeled sulfuryl chloride and application of the aryl F-18 labeled sulfuryl chloride in amine compound labeling. The method takes thiophenol derivative as a labeling precursor, obtains F-18 labeled thiophenol intermediate through photocatalytic aryl F-18 fluorination reaction, and then obtains aryl F-18 labeled sulfuryl chloride through N-chlorosuccinimide oxidation chlorination. The obtained aryl F-18 labeled sulfuryl chloride (4-[ 18 F] fluorobenzenesulfonyl chloride) can occur sulfurylization reaction with various amine compounds at room temperature, and the radiochemical conversion rate is as high as 98%. The application is successfully applied to novel synthesis of AMPA receptor PET imaging agent[ 18 F]2 (the conversion rate is 96%, which is much higher than 13% reported in the literature). The application has the advantages of mild reaction condition, high conversion rate and wide substrate application range, and provides an efficient method for innovative preparation of F-18 labeled PET probes.

The invention belongs to the field of Velciguat synthesis, and particularly relates to a preparation method of Velciguat and an intermediate product thereof. The preparation method of the Velciguat comprises the following steps: (1) reacting aminomalononitrile with methyl chloroformate to generate an intermediate product I; (2) carrying out ring closing on the intermediate product I and formamidine under an alkaline condition to obtain an intermediate product II; (3) carrying out bromination reaction on the intermediate product II and N-bromosuccinimide to obtain an intermediate product III; (4) reacting the intermediate product III with bis (pinacolato) diboron under the action of a catalyst to obtain an intermediate product IV; and (5) carrying out a reaction on the intermediate product IV and 5-fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo [3, 4-b] pyridine to prepare the viriciguat. The method is simple to operate, low in cost and safe in production. The invention also provides the intermediate product obtained by the preparation method.

The invention belongs to the technical field of deuterated organic chemical synthesis, and particularly relates to a synthesis method of deuterated 9-phenyl anthraceneboronic acid-D8, which comprises the following steps of: 1, halogenation reaction: reacting 9-phenyl anthracene-D9, bromo-succinimide (NBS) and triethylamine (TEA) in dichloromethane at low temperature to generate an intermediate 9-phenyl-10-bromoanthracene-D8; step 2, carrying out nucleophilic reaction of forming carbon negative by pulling out bromine with strong in a low-temperature environment of-65 DEG C to-70 DEG C, reacting n-butyllithium with the intermediate 9-phenyl-10-bromoanthracene-D8 in 2-methyltetrahydrofuran to generate 9-phenyl anthracene lithium; then triisopropyl borate is added for a boronation reaction, and the 9-phenyl anthracene boric acid-D8 is obtained after hydrochloric acid hydrolysis and purification. The purity of the deuterated 9-phenyl anthracene boric acid-D8 is greater than or equal to 99.8%, the deuteration rate is greater than or equal to 98%, and the deuterated 9-phenyl anthracene boric acid-D8 is suitable for being used as

The invention discloses a preparation process of 5-bromonicotinic acid, which comprises the following steps: sequentially adding ethyl nicotinate and pinacol borane into a reaction kettle, heating to react, adding N-bromosuccinimide into the reaction kettle, maintaining the reaction temperature, and filtering to remove a byproduct succinimide after the reaction is finished. And carrying out reduced pressure distillation to recover the solvent to obtain the ethyl 5-bromonicotinate. Adding ethyl 5-bromonicotinate into another reaction kettle, adding an alkali solution, heating, stirring for reaction, cooling reaction liquid after the reaction is finished, dropwise adding hydrochloric acid to adjust the pH value, cooling, crystallizing, filtering, washing a filter cake, and drying to obtain a 5-bromonicotinic acid finished product. The total yield gt of the preparation process of the 5-bromonicotinic acid; the HPLC purity is gt; 99%. The process is simple and convenient to operate and easy to implement, raw materials are cheap and easy to obtain, reaction conditions are mild, high-temperature and high-pressure reaction is not needed, and requirements on equipment are reduced. The whole process is safer to the environment, and green and pollution-free production can be realized.

The invention discloses a preparation method and application of a liquid reaction type bromine flame retardant, and belongs to the technical field of flame retardant preparation, and the preparation method comprises the following steps: mixing polypropylene glycol, tetrahydrofuran, N-bromosuccinimide, azodiisobutyronitrile and tetrahydrofuran for reaction, and performing post-treatment to obtain a brominated polyether polyol flame retardant; according to the invention, the prepared brominated polyether polyol flame retardant is also used in thermosetting resin to prepare a flame-retardant resin composition; according to the brominated polyether polyol flame retardant, the balance of high bromine content, high reaction activity and excellent synergism is realized; as a reactive flame retardant, the flame retardant not only can improve the flame retardant property of thermosetting resins such as polyurethane, but also can better retain the inherent physical and mechanical properties of a resin matrix.

The invention discloses a method for synthesizing 3-bromine-9-ethyl carbazole through reactive extrusion. The method comprises the following reaction steps: (1) adding uniformly mixed 9-ethyl carbazole, N-bromosuccinimide and a solid diluent into a solid feeding bin of a double-screw extruder; (2) adjusting the feeding speed and the screw rotating speed of the double-screw extruder, and dropwise adding auxiliary liquid through a peristaltic pump; and (3) collecting the product, dissolving, filtering, evaporating to remove the solvent and the like to obtain the 3-bromine-9-ethyl carbazole. According to the present invention, the double-screw extruder is adopted to efficiently prepare the 3-bromo-9-ethyl carbazole through the reaction extrusion, such that the use amount of the toxic and harmful solvent is substantially reduced, the product yield is improved, and the good application prospect is provided.

This invention relates to the field of pharmaceutical and food flavoring synthesis technology, specifically disclosing a method for preparing 4-ethoxy-3-methoxybenzaldehyde. This method uses... N Using 4-ethoxy-3-methoxybenzyl)methanesulfonamide as a raw material, in an organic solvent, under light conditions, at 30°C, it reacts with... N Chlorosuccinimide (NCS) reacts with deionized water to produce 4-ethoxy-3-methoxybenzaldehyde. This method features mild reaction conditions, requires no expensive reagents or catalysts, does not require the use of hazardous oxidants such as peroxides or oxygen, and is safe and simple to operate.

The application belongs to the technical field of pesticide intermediate preparation, and discloses a preparation method and application of 4-chloro-2,6-dimethylbromobenzene. The method uses 3,5-dimethylphenol as a starting material, and first reacts with p-toluenesulfonyl chloride under alkaline conditions to obtain 3,5-dimethylphenyl p-toluenesulfonate, then performs selective bromination with N-bromosuccinimide in the presence of a free radical initiator to obtain 4-bromo-3,5-dimethylphenyl p-toluenesulfonate, and finally performs a substitution reaction with a chlorine source such as concentrated hydrochloric acid or lithium chloride to obtain the target product 4-chloro-2,6-dimethylbromobenzene; the product can be used for synthesizing pesticides such as methoxypiperidine acetate and dispiro. The method realizes high-selectivity halogenation by regulating the electron cloud distribution of the benzene ring through functional group transformation, has mild reaction conditions, simple operation, avoids high-risk reagents and processes, has high yield, less waste, low cost, and is suitable for industrial production.

The application belongs to the field of vixepiromide synthesis, and particularly relates to a preparation method of vixepiromide and intermediate products thereof. The preparation method of vixepiromide comprises the following steps: (1) reacting aminopropandinitrile with methyl chloroformate to generate an intermediate product one; (2) ring closing the intermediate product one with formamidine under alkaline conditions to generate an intermediate product two; (3) performing bromination on the intermediate product two with N-bromosuccinimide to generate an intermediate product three; (4) reacting the intermediate product three with pinacol diboron under the action of a catalyst to generate an intermediate product four; and (5) reacting the intermediate product four with 5-fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo[3,4-b]pyridine to generate vixepiromide. The application has the advantages of simple operation, low cost and safe production. The application further provides the intermediate products generated in the above preparation method.

The invention provides an ionic liquid-containing lubricating oil composition for a piston type aero-engine, and relates to the technical field of lubricating oil. The composition is prepared from the following components in percentage by weight: 1 to 2 percent of ionic liquid, 0.5 to 2.0 percent of an antioxidant mixture, 0.5 to 1.0 percent of tricresyl phosphate, 0.01 to 0.2 percent of a benzotriazole metal deactivator, 6.0 to 9.0 percent of an ethylene-propylene copolymer viscosity index improver, 3.0 to 6.0 percent of a succinimide ashless dispersant, 10 to 100 ppm of an anti-foaming agent and the balance of base oil, wherein the antioxidant mixture is prepared from the following components in percentage by weight: 0.4 to 1.0 percent of p-diisooctyl diphenylamine and 0.4 to 1.0 percent of lipid antioxidant. According to the piston type aviation lubricating oil composition containing the ionic liquid, the wear resistance, the thermal stability, the low-temperature fluidity and the oxidation resistance of lubricating oil are improved.

The application discloses a chiral thioimine lipid compound and a preparation method and application thereof, and the preparation method comprises the following steps: stirring sulfenamide, isobutyl alcohol, MS, a metal center chiral cobalt (III) complex anion and super-dry tetrahydrofuran at-40 DEG C for 30 minutes, then adding N-iodosuccinimide, and reacting at the same temperature for 36 hours; after the reaction is completed, the reaction is quenched by using an aqueous Na2S2O3 solution, and the chiral thioimine lipid compound is obtained through separation and purification; the chiral thioimine lipid compound prepared by the application provides a robust and practical method for solving the challenging asymmetric problem in sulfur stereochemistry, and opens up a road for a new type of chiral sulfur-containing compound which has a wide application in the fields of medicine and pesticides.

This invention discloses a highly dispersible lubricating oil composition, its preparation method, and a diesel engine oil, belonging to the field of lubricating oil technology. The lubricating oil composition, by mass percentage, comprises: detergent, 1%–6%; dispersant, 1%–8%; corrosion inhibitor, 0.1%–5%; antioxidant, 0.1%–6%; viscosity index improver, 0.1%–4%; base oil, balance; wherein the dispersant is selected from succinimidyl-succinate polymers. The highly dispersible lubricating oil composition and diesel engine oil provided by this invention exhibit excellent dispersing and detergency properties.

The application discloses a succinimide triptycyl compound organic solvent composite nanofiltration membrane and a preparation method thereof, and belongs to the technical field of separation membranes. The application is characterized in that, polyacrylonitrile or polyimide ultrafiltration membrane is used as a base film, after a surface pore preserving agent is removed, the base film is first soaked in an aqueous solution containing a succinimide triptycyl compound, then is soaked in an organic solution containing a polybasic acid chloride to perform an interfacial polymerization reaction, and finally is dried through heat crosslinking to obtain a composite nanofiltration membrane. The composite nanofiltration membrane prepared by the application has high stability in various polar organic solvents, has good selectivity to organic small molecules, and has high solvent permeability, and has high economic value in separation of organic solvent systems in industry.

This invention discloses a eutectic solvent and its preparation, a metal leaching agent, and a metal leaching method. The eutectic solvent is prepared by mixing choline chloride and a sulfonamide compound in a specific ratio; the sulfonamide compound is sulfonamide, 4-amino-N-(aminoiminomethyl)benzenesulfonic acid, or p-aminobenzenesulfonamide. This invention provides a metal leaching agent containing the aforementioned eutectic solvent, which is a transparent liquid prepared from the eutectic solvent and an auxiliary agent. The auxiliary agent is at least one selected from 1,3-dibromo-5,5-dimethylhydantoin, 1,3-dichloro-5,5-dimethylhydantoin, N-chlorosuccinimide, N-bromosuccinimide, chloramine T, and sodium hypochlorite. The eutectic solvent of this invention is an environmentally friendly compound, and the metal leaching agent system containing this eutectic solvent possesses both good oxidizing and coordinating abilities, enabling the leaching of gold and palladium with rapid leaching speed and high extraction rate.

The invention belongs to the technical field of lubricating grease, and discloses a lubricating grease composition and a preparation method thereof, the lubricating grease composition contains base oil, modified graphene and a thickening agent; the modified graphene is prepared by carrying out ball milling on graphene and polyisobutylene succinimide in the presence of supercritical carbon dioxide; relative to 100 parts by weight of the base oil, the content of the modified graphene is 0.005-5 parts by weight. The lubricating grease composition provided by the invention has good stability, lubricity and extreme pressure property.

This invention discloses a method for preparing deuterated 1,2-dibromoethane, comprising the following steps: (1) adding tetradeuterium glycol, N-bromosuccinimide, and solvent into a reaction vessel; (2) controlling the temperature inside the reaction vessel at -5 to 20°C, and then adding a mixture of triphenylphosphine and solvent dropwise into the reaction vessel; (3) after the dropwise addition is completed, restoring the reaction vessel to room temperature, and controlling the reaction time to 0.5 to 1.5 h to obtain a product containing deuterated 1,2-dibromoethane. The reaction temperature of this invention is at room temperature, the reaction operation is simple, it meets the requirements of green chemistry, and it can be industrialized. Furthermore, the purity of deuterated 1,2-dibromoethane is above 98 wt%, and the yield of deuterated 1,2-dibromoethane is above 60 wt%.

The invention provides a method for recycling and regenerating chlorosuccinimide, and belongs to the technical field of resource recycling. The method comprises the following steps: decoloring the mother liquor after reaction, adding sulfide to enable metal palladium to form palladium sulfide precipitate, performing chlorination reaction on filtrate, ferrous chloride and phosphorus oxychloride, and performing extraction and back extraction to obtain chlorosuccinimide, so that the chlorosuccinimide is recycled and regenerated. The result of the embodiment shows that the melting point of the chlorosuccinimide obtained by the method disclosed by the invention is consistent with a literature value.

The application discloses a bipolar polymer semiconductor material containing difluoro-substituted indathrene and a preparation method and application thereof. N The copolymerization of the obtained copolymer monomer and 5,5'- (bistrimethyltinyl) -2,2'-dithiophene or (E) -1,2- (5- (bistrimethyltinyl) -thiophene-2-yl) ethylene, a centrosymmetric monomer, through a bromination reaction of bromo-succinimide to obtain a novel bipolar polymer semiconductor material containing difluoro-substituted indathrene with a D-A configuration. The synthesis route of the application is simple and efficient, raw materials are easy to obtain, the cost is low, the universality is high, and the repeatability is good. The material has the advantages of good solubility, excellent thermal stability and strong absorption spectrum range. The bipolar polymer semiconductor material prepared by the application is used as an active layer material, and an organic field effect transistor device prepared by the application has excellent electrical performance. The material has broad commercial prospects in organic thermoelectricity, organic field effect transistors, organic logic complementary circuits and other optoelectronic devices.

This invention discloses a method for preparing bromobenzothiophene, relating to the field of organic synthesis. In the preparation of bromobenzothiophene, N-bromosuccinimide is first purified by recrystallization; benzo[b]thiophene is mixed evenly with acetonitrile, and then the purified N-bromosuccinimide is added in batches while stirring. Finally, deionized water is added to the reaction solution, followed by stirring, filtration, washing, and drying to obtain 3-bromobenzo[b]thiophene. The method for preparing bromobenzothiophene provided by this invention reduces the generation of toxic byproducts due to solvent substitution, resulting in a higher yield of bromobenzothiophene. Furthermore, the preparation method provided in this application can be carried out at a lower temperature, saving energy.

The application relates to the field of printed circuit board production processes, in particular to an environment-friendly alkaline degreasing agent for non-conductive printed circuit board materials, a production process and application. The environment-friendly alkaline degreasing agent is composed of the following raw materials: 70-90 g / L of an environment-friendly alkali source, 3-8 g / L of a surfactant, 5-12 g / L of a stabilizing auxiliary agent, 1-8 g / L of modified citrate, 0.1-0.5 g / L of an antioxidant and the balance of water; the environment-friendly alkali source is a mixture of multiple kinds of sodium silicate, sodium hexametaphosphate, potassium hydroxide, trisodium phosphate, monoethanolamine and sodium gluconate, wherein at least one kind is potassium hydroxide; and the stabilizing auxiliary agent is composed of boronized polyisobutylene succinimide, branched polyether and hydrophilic modified cellulose nanocrystals. The above technical scheme can achieve uniformity and good degreasing effect in batch degreasing process, and guarantees the quality and production efficiency of products.

The present application relates to a kind of preparation of deuterated 9-bromoanthracene method, wherein the preparation method includes according to the following steps is reacted: (1) dichloromethane, deuterated anthracene is mixed in reactor;(2) bromo succinimide NBS is added;(3) reduced pressure distillation;(4) separation and purification are obtained.

The invention discloses a method for continuously synthesizing 5, 5 '-dibromo-2, 2'-bithiophene through twin-screw extrusion, which comprises the following reaction steps: (1) adding 2, 2 '-bithiophene, N-bromosuccinimide and a solid diluent which are uniformly mixed into a feeding bin of a twin-screw extruder; (2) adjusting the feeding speed and the screw rotating speed of the double-screw extruder; and (3) collecting the product, dissolving, filtering, evaporating to remove the solvent and the like to obtain the 5, 5 '-dibromo-2, 2'-bithiophene. According to the present invention, the solvent-free continuous efficient preparation of 5, 5 '-dibromo-2, 2'-bithiophene is achieved by using the twin-screw extrusion technology, the method is green and environmentally friendly, the product yield is increased, and the method has good application prospects.

This invention belongs to the field of organic synthesis, specifically relating to a method for preparing 2,6-dichlorofluorobenzene, comprising: phenol and a chlorination reagent. N Chlorosuccinimide undergoes a chlorination reaction in the presence of a Pd catalyst and 1,10-phenanthroline-5,6-dione to produce 2,6-dichlorophenol. 2,6-Dichlorophenol, fluorinating agent NFSI, photocatalyst 4-CzIPN, and an ionic liquid undergo a deoxyfluorination reaction under blue LED irradiation to produce 2,6-dichlorofluorobenzene. This invention offers high product yield and purity, mild reaction conditions, and avoids the use of hazardous raw materials, making it suitable for industrial production.

The invention relates to the technical field of rolling oil, and particularly discloses low-residual-carbon high-temperature-resistant hot rolling oil and a preparation method thereof, and the rolling oil comprises the following components by weight percent: 36-48% of mineral oil; 8-12% of vegetable oil; 12-18% of synthetic ester group; 0.4%-0.7% of an antioxidant; 1.6%-1.9% of an extreme pressure agent; 28-40% of special synthetic ester; 0.4-1.0% of an emulsifier; 0.8%-1.6% of a nano reinforcing agent; the nano reinforcing agent is a combination of nano silicon dioxide and nano boron nitride, the dispersing agent is polyisobutylene succinimide, and the rolling oil provided by the invention has the advantages of low residual carbon content, high extreme pressure property, excellent high temperature resistance and thick lubricating film.

This invention discloses a method for preparing functionalized polyolefins, belonging to the field of polymer modification technology. The method includes the following steps: homogenizing a polyolefin, a grafting monomer, and a high-valent iodine compound, followed by heating to obtain the functionalized polyolefin; wherein the grafting monomer is selected from at least one of N-hydroxyphthalimide and its derivatives, and N-hydroxysuccinimide and its derivatives. This method uses a high-valent iodine compound as an initiator, which preferentially activates the polyolefin molecular chain and forms a pre-bonded complex with the grafting monomer. This significantly inhibits the non-selective β-fracture degradation and inter-chain crosslinking of the polyolefin backbone caused by free radicals, maintains the stability of the base molecular weight, and achieves efficient grafting of the grafting monomer.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of triazolone-14C. Comprising the following steps: synthesizing phenol-14C: preparing a system A: adding water and concentrated sulfuric acid into a single-mouth bottle and stirring; performing liquid separation on aniline hydrochloride-14C and a saturated sodium bicarbonate solution, performing extraction, adding an organic phase into the system A, performing reaction concentration, dropwise adding sodium nitrite, adding methylbenzene, and performing reaction at 100 DEG C; extracting, drying, filtering, concentrating, and passing through a chromatographic column; the preparation method comprises the following steps: synthesizing 4-chlorophenol-14C, namely dropwise adding N-chlorosuccinimide into 4-chlorophenol-14C, p-toluenesulfonic acid and acetonitrile, and reacting completely; extracting, drying, filtering, concentrating, and passing through a chromatographic column; 4-chlorophenol-14C, ethyl acetate, 1, 2, 4-triazole, potassium carbonate and 600 polyethylene glycol are synthesized, 1, 1-dichloropinacolone is dropwise added, and a reaction is conducted at the temperature of 85 DEG C; after the reaction is finished, cooling to room temperature, extracting, drying, filtering, concentrating, and passing through a chromatographic column; the total yield of the three steps is basically maintained between 60% and 85%, the synthetic reaction conditions are simple, and the yield is high.

The invention relates to the technical field of lubricating oil, in particular to marine four-stroke methanol engine lubricating oil and a preparation method and application thereof. The marine four-stroke methanol engine lubricating oil is prepared from the following components in parts by weight: 80 to 95 parts of mineral oil, 1 to 5 parts of salicylate, 0 to 2.5 parts of sulfurized alkyl phenate, 3.5 to 4.5 parts of succinimide, 0.5 to 1.2 parts of zinc dioctyl dithiophosphate, 0.1 to 0.5 part of zinc butyl octyl dithiophosphate, 0 to 0.5 part of amine type antioxidant and 0.01 to 0.1 part of anti-foaming agent. The low-ash-content alkali-retaining agent has the advantages of being good in alkali-retaining performance, oxidation resistance and corrosion resistance and low in ash content.

This invention relates to a method for preparing 2',4-dichloro-2-aminodiphenyl ether, belonging to the field of chemical synthesis technology. The preparation method is as follows: S1, m-dinitrobenzene undergoes selective hydrogenation to obtain m-nitroaniline; S2, in a solvent, m-nitroaniline reacts with N-chlorosuccinimide to obtain 2-chloro-5-nitroaniline; S3, 2-chloro-5-nitroaniline, o-nitrophenol, a base, and a solvent undergo a co-heated reaction to obtain 2',4-dinitro-2-aminodiphenyl ether; S4, 2',4-dinitro-2-aminodiphenyl ether is dissolved in a solvent, and FeCl3 solution, sodium chloride, and Oxone are added. The reaction is catalyzed under ultraviolet light to obtain 2',4-dichloro-2-aminodiphenyl ether. The preparation method of this invention uses readily available raw materials, has good reaction efficiency, produces less waste, is cleaner and more environmentally friendly, and has a high conversion rate, making it suitable for industrial application.