275 results about "Thionyl chloride" patented technology

The invention provides a polyurethane material for leaking stoppage of a coal mine and a preparation method of the polyurethane material, and belongs to the technical field of polyurethane. The preparation method comprises the following steps: preparing melamine formaldehyde resin balls and ZnAl-LDHs, mixing and reacting the melamine formaldehyde resin balls and the ZnAl-LDHs to prepare LDH-MF composite balls, dipping in an iron salt solution, calcining to prepare composite balls, chloridizing with thionyl chloride, reacting with an ionic liquid and hyperbranched polyester to prepare IL / G composite balls, mixing with polyether polyol and a catalyst, adding into water, adding a foaming agent and silicone oil, heating, stirring and mixing, transferring into a mold, and carrying out extrusion molding to obtain a finished product. And adding diisocyanate, foaming, cooling to room temperature, drying and curing to obtain the polyurethane material for leaking stoppage of the coal mine. The prepared polyurethane material for leaking stoppage of the coal mine has good mechanical property, high temperature resistance and antibacterial property, good flexibility, good antistatic property and obviously improved flame retardance, and has a wide application prospect.

The invention belongs to the technical field of sulfonamide synthesis, and particularly relates to a green and environment-friendly sulfonamide amidation preparation method. Comprising the following steps: adding chlorosulfonic acid into a reactor, stirring, heating, adding o-nitrochlorobenzene, carrying out staged heat preservation, cooling, and adding thionyl chloride to obtain 2-nitro-4-chlorine sulfonate-chlorobenzene; the method comprises the following steps: separating and filtering 2-nitro-4-chlorine sulfonate-chlorobenzene, adding ammonia water, stirring, preserving heat, and carrying out filter pressing to obtain 2-nitro-4-amine sulfonate-chlorobenzene; the preparation method comprises the following steps: adding liquid caustic soda into 2-nitro-4-amine sulfonate-chlorobenzene, stirring, heating, and adjusting the pH value to obtain 2-nitro-4-amine sulfonate-phenol; the method comprises the following steps: adding water, a catalyst and hydrazine hydrate into 2-nitro-4-amine sulfonate-phenol, heating, stirring, and carrying out filter pressing to obtain 4-sulfonamide-2-amino-phenol. According to the preparation method of sulfonamide, generated tail gas is subjected to falling film absorption treatment, and the product prepared by the preparation method is high in purity.

The invention provides a method for producing 4, 4 '-dichlorodiphenyl sulfone by continuous reaction of a microchannel reactor, which comprises the following steps: uniformly mixing thionyl chloride and aluminum chloride to obtain a solution A; uniformly mixing hydrogen peroxide and glacial acetic acid to obtain a solution B; a first feeding pump and a second feeding pump are adopted for conveying chlorobenzene and a solution A into a first silicon carbide micro-channel reactor for reaction, an outlet of the reactor is connected with a gas-liquid separator, through separation, a gas phase is used for preparing a byproduct hydrochloric acid, and a liquid phase is a chlorobenzene solution of 4, 4 '-dichlorodiphenyl sulfoxide; and continuously conveying the chlorobenzene solution of 4, 4 '-dichlorodiphenyl sulfoxide to the second silicon carbide microchannel reactor by adopting a third feeding pump, and meanwhile, conveying the solution B to the second silicon carbide microchannel reactor by adopting a fourth feeding pump for reaction to prepare 4, 4'-dichlorodiphenyl sulfone. Compared with the prior art, the micro-channel reactor is used for continuous production, the mass and heat transfer effect is good, impurity generation is effectively inhibited, and the reaction time is shortened.

The invention belongs to the technical field of synthesis of organic intermediates, and particularly relates to a synthesis method and a synthesis device of benzenesulfonyl fluoride. The synthesis method of the benzenesulfonyl fluoride comprises the following steps: firstly, adding hydrogen fluoride and sulfuryl chloride into a premixer, enabling the hydrogen fluoride and the sulfuryl chloride to sequentially pass through tubular reactors a, b and c, enabling the hydrogen fluoride and the sulfuryl chloride to enter a terminal reaction kettle for mixing reaction, controlling gas-liquid two-phase mixing reaction through the terminal reaction kettle and a vertical condenser a to prepare sulfuryl fluoride chloride, then mixing the sulfuryl fluoride chloride, benzene and a catalyst, and finally adding the benzenesulfonyl fluoride into the premixer to obtain the benzenesulfonyl fluoride. The method comprises the following steps: adding benzenesulfonyl fluoride into a sulfonation reaction kettle for reaction, controlling the sulfonation reaction through the sulfonation reaction kettle and a vertical filler b to obtain a mixed reaction solution, finally distilling the mixed reaction solution, and collecting fractions to obtain benzenesulfonyl fluoride. The synthesis method of the benzenesulfonyl fluoride provided by the invention is low in reaction condition requirement, stable, easy to control, low in unit consumption and easy in subsequent treatment, and the prepared benzenesulfonyl fluoride is high in yield and high in purity. The invention also provides a synthesis device adopted by the synthesis method of benzenesulfonyl fluoride.

The invention is suitable for the technical field of fine chemical engineering, and provides a synthesis method of sulpiride impurity 2-hydroxy-5-sulfanilamide benzamide, which comprises the following specific steps: Step 1, taking salicylic acid as a raw material, taking DMF as a catalyst, and carrying out acylation reaction with thionyl chloride to obtain acylation liquid, and entering the next process; 2, ammoniating the acylation liquid with ammonia water at a low temperature to obtain salicylic acid formamide, and drying to obtain an intermediate 1; 3, TMS-Cl is used for protecting phenolic hydroxyl groups, then chlorosulfonic acid is dropwise added, a chlorosulfonation reaction is carried out, and an intermediate 2 solution is obtained after the reaction is completed; and Step 4, dropwise adding the solution of the intermediate 2 into stronger ammonia water for reaction, carrying out suction filtration, and recrystallizing with ethanol to obtain the sulpiride impurity 2-hydroxy-5-sulfanilamide benzamide. The route synthesis is simple, and the quality can reach 95% or above; in addition, the method has the advantages of cheap and easily available raw materials, mild reaction conditions, low energy consumption, simple process structure, easy operation and the like.

The invention discloses a preparation method of 3-quinuclidinone hydrochloride, which comprises the following steps: carrying out temperature control reaction on 4-picolinic acid and chloroacetic acid under alkaline water conditions to obtain an aqueous solution of a compound a, and directly entering the next reaction without post-treatment after the reaction is finished; adding a reducing agent alkaline water system into the aqueous solution of the compound a, controlling the temperature to react, controlling the temperature to adjust the pH value to 5-5.5 after the reaction is finished, extracting with n-butyl alcohol, and drying to obtain an n-butyl alcohol solution of a compound b, and directly entering the next reaction step; wherein the reducing agent is one of sodium borohydride and potassium borohydride; dropwise adding thionyl chloride into an n-butyl alcohol solution of the compound b, controlling the temperature to react after dropwise adding is ended, and concentrating to remove the solvent and unreacted thionyl chloride after the reaction is ended, so as to obtain a compound c; carrying out Dieckmann condensation reaction on the compound c at controlled temperature under the condition of organic alkali by using toluene as a solvent, carrying out hydrochloric acid quenching reaction after the reaction is finished, and directly carrying out next-step reaction after extracting and removing impurities from a water phase containing a hydrochloride solution of a compound d by using toluene; and carrying out a decarboxylation reaction on the compound d in a hydrochloric acid aqueous solution at controlled temperature, after the reaction is finished, adjusting the pH value to 10-13, extracting, and salifying to obtain a target compound TM, namely 3-quinuclidinone hydrochloride. The preparation method of 3-quinuclidinone hydrochloride provided by the invention has the advantages of economical and easily available raw materials, mild reaction conditions, efficient reaction, simple operation and low cost, and is suitable for industrial application.

This invention provides a method for preparing and applying a highly insecticidal diamide compound, relating to the chemical and pesticide fields. The method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; and, during the reaction under a hydrogen atmosphere, determining the reaction temperature and hydrogen flow rate in each hydrogenation reaction zone based on the concentration of compound B; reacting compound C with paraformaldehyde to obtain compound D; chlorinating 3-chloro-4-fluorobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound E; and amide condensing compound E with compound D to obtain the novel diamide compound of this invention. The diamide compound of this invention exhibits excellent insecticidal effects when used in pesticide compositions.

The invention provides a preparation method of fluoride ether bacteria amide, which comprises the following steps: dissolving pentafluorobenzonitrile in a solvent, dropwise adding a sodium methoxide solution at-10-30 DEG C for 2-15 hours, continuing to carry out heat preservation reaction for 0.5-2 hours after dropwise adding, and carrying out post-treatment to obtain 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile; the preparation method comprises the following steps: jointly dissolving 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile, 3-chloro-5-(trifluoromethyl) pyridine-2-yl) methanol and a catalyst acid in a solvent, reacting at 50-110 DEG C for 5-32 hours, and performing post-treatment on the obtained reaction liquid to obtain fluoride ether bacteria amide, according to the method, sodium methoxide and pentafluorobenzonitrile which are low in price and easy to obtain are subjected to etherification reaction, thionyl chloride and bis (trichloromethyl) carbonate are not used, the green chemical principle is met, and the method has the advantages of being short in step, safe and easy to operate and the like, so that the method has high implementation value and practical production applicability.

The present invention provides a thiadiazole compound containing a hindered phenol group, a preparation method thereof and its use in the field of lubricating oil additives. The preparation method of the thiadiazole compound containing a hindered phenol group comprises the following steps: mixing a carboxylic acid compound containing a hindered phenol group with thionyl chloride, removing impurities under reduced pressure to obtain an acyl chloride compound containing hindered phenol; stirring and mixing 2-mercapto-5-amino-1,3,4-thiadiazole with a halogenated hydrocarbon compound, filtering, washing and drying to obtain a 2-mercapto-5-amino-1,3,4-thiadiazole derivative; adding a hindered phenol acyl chloride compound, 2-mercapto-5-amino-1,3,4-thiadiazole derivative and an alkaline additive to an organic solvent, washing, drying and purifying to obtain a thiadiazole compound containing a hindered phenol group. The thiadiazole compound containing a hindered phenol group is an antioxidant, extreme pressure and anti-wear additive, which can be applied to synthetic ester lubricants and has a good antioxidant, extreme pressure and anti-wear effect.

This invention discloses a magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd, its preparation method, and its applications. Using an amino alcohol as a starting material, an imidazole derivative containing a hydroxyl group on the N-substituent is obtained through a condensation and ring-closing reaction. This derivative is then subjected to substitution reactions with thionyl chloride and cyclohexanethiol sequentially to obtain an imidazole derivative containing a thioether on the N-substituent. This derivative is then reacted with 1,3-dibromopropane to obtain an N-bromopropyl-N'-cyclohexane thioether-substituted imidazole bromium salt. This salt is then reacted with Pd(OAc)₂ or PdCl₂ via a direct metallization reaction to obtain the N-bromopropyl-substituted thioether-chelated nitrogen heterocyclic carbene palladium complex NHC-Pd. The NHC-Pd complex is then reacted with amino-functionalized magnetic nanoparticles (MNPs-NH₂) to prepare the magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd. It not only possesses the activity of homogeneous nitrogen heterocyclic carbene palladium catalysts, but also has a simple synthesis method, high yield, and is easy to separate and reuse in catalytic C-C bonding reactions, showing good application prospects in the field of catalysis.

The invention discloses a solvent removal process and a crude product post-treatment method in isophthaloyl chloride / paraphthaloyl chloride production, and belongs to the technical field of chemical processes. A three-stage gradient condensation system is adopted, circulating water, chilled water and chilled saline water are respectively introduced, the recovery rate of thionyl chloride is improved, thionyl chloride is prevented from entering a subsequent vacuum unit, the equipment failure rate is reduced, and the annual overhaul frequency is reduced. A top condenser is arranged, hot water at the temperature of 50-55 DEG C (suitable for producing isophthaloyl dichloride) or hot water at the temperature of 85-90 DEG C (suitable for producing paraphthaloyl dichloride) is adopted as a cooling medium, so that isophthaloyl dichloride / paraphthaloyl dichloride is efficiently captured, and coagulum is thoroughly prevented from entering a subsequent system and blocking equipment and pipelines.

The invention belongs to the field of organic chemical synthesis, and particularly relates to a synthesis method of triaryl sulfonium salt, which comprises the following steps: (1) dissolving a catalyst: dissolving the catalyst in an organic solvent in a preparation kettle in advance to form a uniform solution; and (2) continuous feeding and reaction: enabling reactants thionyl chloride and an aromatic hydrocarbon derivative and the catalyst-containing solution obtained in the step (1) to pass through a continuous reactor at a controllable flow rate, firstly carrying out Friedel-Crafts acylation reaction in an all-solvent system, then heating to carry out addition reaction, and finally obtaining the triaryl sulfonium salt. According to the invention, the problem of solid-liquid non-uniformity is eliminated, and the reaction efficiency and reproducibility are improved; the reaction is fast and uniform, and local overheating and out-of-control risks are avoided.

This invention belongs to the field of insecticide technology, specifically relating to a diamide compound, its preparation method, intermediate preparation equipment, and applications. The preparation method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride in the presence of dimethylformamide to generate compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; substituting compound C with formaldehyde to obtain compound D; and condensing compound D with 3,5-dichloro-4-fluorobenzoyl chloride to obtain the diamide compound. The beneficial effects of this invention are: the diamide compound solves the problem of insecticide resistance and possesses high insecticidal activity, exhibiting good insecticidal effect at low doses. Furthermore, the preparation method uses mild reaction conditions, produces few byproducts, and has a high reaction yield, reducing raw material loss and thus lowering production costs.

The invention discloses a system and method for comprehensive energy utilization of a thionyl chloride catalyst. The system comprises a thionyl chloride catalyst, a heat exchanger, a lithium bromide unit for cooling pure water, and a chilled water system. The outlet end of the thionyl chloride catalyst is connected to the heat exchanger via a pipeline, and gas with a certain amount of heat at the outlet of the thionyl chloride catalyst is directed into the heat exchanger. Pure water is provided in the heat exchanger for continuously passing through the heat exchanger to absorb heat in the gas. The output end of the heat exchanger is connected to the lithium bromide unit via a pipeline, and the output end of the lithium bromide unit is connected to the chilled water system. The invention overcomes the shortcomings of the prior art, recycles energy, reduces production costs, and significantly improves production efficiency. At the same time, the entire production process is optimized for reaction efficiency and material utilization, thereby increasing the economic benefits of the enterprise and having high social use value and application prospects.

The invention discloses a preparation method of a continuously-produced lithium thionyl chloride composite carbon electrode, and relates to the technical field of battery production, and the preparation method comprises the following steps: pre-pressing acetylene black, uniformly mixing the pre-pressed acetylene black with adhesive micro-powder to form powder, and carrying out three working procedures of mixing, rolling to form a film and rolling to fit the film on the powder at the temperature of 80-200 DEG C in sequence to finish fibration, so as to obtain the lithium thionyl chloride composite carbon electrode. The lithium thionyl chloride composite carbon electrode is obtained. The preparation process is free of a baking procedure, energy is saved, emission is reduced by 50% or above, and the production period is shortened to 1 day from 3 days of wet-process film rolling or 2 days of semi-dry powder net loading; and a first-grade flammable and explosive organic solvent with poor production safety is not needed, so that the safety risk and the production cost are reduced. The growth suitability of the bonding strength of each section of fibration is controlled through process design, the purpose of film combination after film formation is achieved, a thick electrode required by higher capacity can be prepared, and the adverse effects of net separation, floating powder and the like are avoided.

The invention relates to the technical field of synthesis of ester compounds, in particular to a preparation method of an ester compound based on a sulfur trioxide compound. The method comprises the following steps: by taking a sulfur trioxide compound as a carboxylic acid activating agent and taking a carboxylic acid-containing compound and a hydroxyl-containing compound as raw materials, carrying out esterification reaction at room temperature in a reaction system of an alkali substance, a sodium salt stabilizer and a solvent, activating carboxylic acid by sulfur trioxide to form an active intermediate, and reacting the active intermediate with hydroxyl to generate an ester compound. The ester compound based on the sulfur trioxide compound is obtained, and sodium sulfate precipitate is obtained at the same time. According to the method, acyl chloride, thionyl chloride or unstable condensation reagents with high corrosivity are not used in the reaction, chlorine-containing wastewater is not generated, the reaction is carried out at room temperature, heating or high temperature is not used, the reaction condition is mild, the product is easy to separate, the use of organic solvents can be effectively reduced through post-treatment, and the product yield is relatively high.

The invention relates to the technical field of fine chemical engineering, in particular to a method for recycling kettle residues in the production process of bis (chlorosulfonyl) imide. The innovative method focuses on effective recovery and reutilization of the kettle residues generated in the existing production process for the first time, so that many challenges such as high difficulty in treatment of the kettle residues, high environmental pollution risk, strong substance corrosivity and operation danger are successfully handled; the atom economic efficiency of a synthesis path of sulfamic acid, chlorosulfonic acid and thionyl chloride is also obviously improved. The comprehensive yield of the method can reach up to 99%, and the purity of the bis (chlorosulfonyl) imide product prepared through the kettle residue recovery reaction exceeds 98.5%, so that the strict requirement of downstream application on the purity of the bis (chlorosulfonyl) imide product is fully met.

A method includes providing, within an etch chamber, a base structure including a target layer disposed on a substrate, and an etch mask disposed on the target layer, dry etching, within the etch chamber, the target layer using thionyl chloride to obtain a processed base structure, and after forming the plurality of features. The processed base structure includes a plurality of features and a plurality of openings defined by the etch mask. The method further includes removing the processed base structure from the etch chamber. In some embodiments, the target layer includes carbon. In some embodiments, the dry etching is performed at a sub-zero degree temperature.

The utility model discloses a continuous reaction device for producing bis (chlorosulfonyl) imide, which belongs to the technical field of chemical equipment and comprises a horizontal reaction tank and a heat preservation tank, a feed port of the reaction tank is connected with a mixed feed liquid pipe, and a discharge port of the reaction tank is connected with the heat preservation tank through a conveying component; heating layers are arranged outside the reaction tank and the heat preservation tank, a plurality of communicated areas are arranged in the reaction tank and the heat preservation tank, a stirrer is arranged in each area, and a chlorosulfonic acid feeding hole is formed in the top of each area of the reaction tank; a discharge hole of the heat preservation tank is connected with the distillation device; exhaust pipes and condensation reflux assemblies are arranged at the tops of the reaction tank and the heat preservation tank. The chlorosulfonic acid is added into each area of the reaction tank in a multi-drop mode, the reaction tank heats materials through the heat preservation layer to ensure the temperature needed by reaction, and the materials enter the heat preservation tank to be subjected to continuous heat preservation to ensure full reaction of the materials; thionyl chloride in gas exhausted from the reaction tank and the heat preservation tank is cooled and recycled through the condensation backflow assembly, the production efficiency is improved, raw material waste is reduced, and the production cost is reduced.

A method of ALE etching of a III-V material including the following steps: a) placing in an enclosure a structure including a layer of III-V material, b) implementing, in the enclosure, at an etching temperature, one or more times the following ALE cycle: oxidizing a surface of the layer of III-V material with an oxidizing gas, whereby an oxide layer is formed, purging the enclosure with an inert gas flow, exposing the formed oxide layer to thionyl chloride vapor to etch the oxide layer, and purging the enclosure with an inert gas flow.

The present invention discloses a preparation method of mesotrione, and the method steps are as follows: S1: Under the protection of an inert gas, 3-chloro-2-methylbenzenemethanethiol, phosphorus oxychloride, a composite catalyst and an organic solvent are mixed and reacted. After the reaction is completed, 2-chloro-3-methyl-4-methylthiophenylaldehyde is obtained through separation and vacuum distillation; 2-chloro-3-methyl-4-methylthiophenylaldehyde is mixed with sodium tungstate dihydrate and methanol, and hydrogen peroxide is added for reaction. After the reaction, 2-chloro-3-methyl-4-methylsulfonylbenzoic acid is obtained through filtration; S2: Preparation of 2-chloro-3-(2,2,2-trifluoroethoxy)methyl-4-methylsulfonylbenzoic acid; S3: 2-chloro-3-(2,2,2-trifluoroethoxy)methyl-4-methylsulfonylbenzoic acid is mixed and reacted with thionyl chloride and dichloroethane, and the reaction product is further reacted with 1,3-cyclohexanedione, triethylamine and samarium trichloride to prepare mesotrione. The present invention simplifies the preparation route of mesotrione, the preparation process is more green and safe, and the yield of mesotrione is higher.

The invention discloses a degradable environment-friendly fiber and a preparation method thereof, and relates to the field of fibers. When the degradable environment-friendly fiber is prepared, triethyl phosphite firstly reacts with 3-(2-bromoethyl) thiophene and then reacts with dimethyl terephthalate and ethylene glycol, and modified polyester is prepared; the preparation method comprises the following steps: enabling chitosan oligosaccharide to react with 4-hydroxy-3-pyridylaldehyde, thionyl chloride and 2-(dimethylaminomethyl) thiophene in sequence, so as to prepare functionalized chitosan oligosaccharide; mixing the functionalized chitosan oligosaccharide, zinc acetate and modified polyester, and performing melt spinning to obtain composite fibers; mixing thiophene, ferric chloride and trichloromethane to prepare a thiophene solution; and immersing the composite fiber in a thiophene solution, and drying to obtain the degradable environment-friendly fiber. The degradable environment-friendly fiber prepared by the invention has excellent flame retardance, antibacterial property, antistatic property and light aging resistance.

The invention discloses a preparation method of an LH-1801 key intermediate, and belongs to the field of medicine synthesis. The preparation method comprises the following steps: enabling SM1 and NBS to react in an acid solution to obtain a compound 1; catalyzing the compound 1 and NBS in an organic solvent in the presence of a catalyst to obtain a compound 2; catalyzing the compound 2 and thionyl chloride in the presence of a catalyst to obtain a compound 3; performing Friedel-Crafts reaction on the compound 3 and 2-ethylthiophene in an organic solvent under the catalysis of a catalyst to obtain a compound 4; reacting the compound 4 with triethyl silane and boron trifluoride diethyl etherate in an organic solvent to obtain a compound 5; reacting the compound 5 with a salt solvent in an organic solvent to obtain a compound 6; and finally, reacting the compound 6 with an alkali solvent in an organic solvent to obtain a compound 7, namely the LH-1801 intermediate. According to the method, 2-chloro-4-methyl benzoic acid is used as a starting material, the intermediate steps are simple and mild reactions, the operation difficulty is low, the reaction risk is low, and the method is suitable for industrial production.

The present invention relates to a 13 C. 18 The synthesis method of trifluoroacetic acid with O stable isotope double labeling is as follows: firstly, trifluoroacetic acid is dissolved in a solvent, metal ions are added, and 13 C-labeled carbon dioxide, react to obtain a reaction solution, then separate and dry the reaction solution to obtain 13 C-enriched trifluoroacetic acid, and finally 13 C-enriched trifluoroacetic acid is dissolved in an aprotic solvent, thionyl chloride is added, stirred for reaction, and then a catalyst and oxygen 18 water are added, heated for reaction, and the reaction product is separated to obtain 13 C. 18 O stable isotope double labeled trifluoroacetic acid is the target product. Compared with the prior art, the present invention has a simple reaction process, a simple post-processing process, and a high yield. 13 The C isotope abundance is over 98%. 18 The O isotope abundance is over 97%.

The invention relates to the technical field of organic synthesis, in particular to a method for preparing 4-nitro-N-phenylbenzamide by a one-pot process, which comprises the following steps: under the protection of inert gas, adding an inert solvent, p-nitrobenzoic acid and a composite catalyst into a reactor, and heating to dissolve, the composite catalyst comprising NFM and TPPO; slowly adding thionyl chloride into a reaction system for acylation reaction; then slowly adding aniline into the reaction system to carry out condensation reaction; and after the reaction is finished, carrying out post-treatment to obtain the 4-nitro-N-phenylbenzamide. According to the method, one-pot reaction can be realized, and high-risk intermediates do not need to be separated. In the composite catalyst, NFM efficiently catalyzes acylating chlorination, and TPPO stabilizes an acyl chloride intermediate and promotes condensation, so that the reaction is performed efficiently, stably and highly selectively, and the product is high in yield and purity. And the catalyst is easy to recycle, and the process is green, safe, economical and suitable for industrial production.

The invention discloses a substituted quinoline compound and a preparation method and application thereof.The preparation method includes the steps that thionyl chloride and a specific intermediate react, DCM and other solvents are adopted, and pyridine, polyphosphoric acid, ethyl alcohol, acetyl chloride and other reagents are used in the reaction process. The structure of the obtained product is confirmed by a nuclear magnetic hydrogen spectrum, bactericidal activity tests are carried out on the obtained 29 target products, and the results show that the compound has a significant inhibition effect on a variety of plant pathogens at a concentration of 50 ppm, and especially shows excellent bactericidal activity in the aspects of pyricularia grisea, sclerotinia sclerotiorum and the like. In addition, the compounds have certain herbicidal activity.

The invention provides a lithium thionyl chloride primary battery and a preparation method thereof. The lithium thionyl chloride primary battery comprises a lithium metal negative electrode, a diaphragm, a positive electrode and thionyl chloride electrolyte; wherein the surface of the lithium metal negative electrode is provided with a nano metal coating and / or the thionyl chloride electrolyte comprises a phthalocyanine metal complex. According to the invention, the nano-metal coating can protect the lithium metal negative electrode from being corroded by thionyl chloride, so that the battery is prevented from self-discharge during a storage period or an idle period of intermittent discharge, and lithium ions can be promoted to migrate to the positive electrode; the phthalocyanine metal complex can preferably enable the reduction reaction of thionyl chloride to be carried out more efficiently, the discharge voltage of the battery is improved, meanwhile, the resistance of the electrolyte can be reduced, and the high-current discharge performance of the lithium thionyl chloride primary battery is improved. Therefore, the lithium thionyl chloride primary battery can quickly respond when discharging is needed, capacity loss is avoided when discharging is not needed, and the overall discharging capacity of the battery can be improved.

The invention discloses a novel bismuth-based chelate CT contrast agent and a preparation method and application thereof. The synthesis method comprises the following steps: reacting 2, 6-pyridine dimethyl carbinol with thionyl chloride to obtain 2, 6-bis (chloromethyl) pyridine; the preparation method comprises the following steps: carrying out a heating reaction on 2-(4-methylphenyl)-1, 2, 4-triazine-2-ketone, N, N ', N'-tri (p-toluenesulfonyl) diethylenetriamine and an inorganic base in a solvent, and carrying out concentrated sulfuric acid deprotection to obtain an intermediate pyclen; the preparation method comprises the following steps: heating and reacting pyrene and halogenated carboxylic ester in a polar organic solvent under an alkaline condition, and hydrolyzing to obtain a ligand product; and heating and chelating the ligand product and a bismuth agent to prepare the target bismuth-based chelate. Laboratory large-scale preparation of the small-molecule bismuth-based chelate CT contrast agent is achieved, and the prepared nonionic contrast agent has low osmotic pressure, high stability, high water solubility and good biological safety and is used for CT imaging of digestion, urinary and circulatory systems.

This invention provides a method for preparing high-purity olaparib, belonging to the field of pharmaceutical synthesis technology. The method uses dimethyl (3-oxo-1,3-dihydroisobenzofuran-1-yl)phosphate as the starting material, reacting it with compound 2 via a Wittig reaction to generate compound 3. Compound 3 reacts with hydrazine hydrate to generate compound 4. Compound 4 is hydrolyzed and acidified to give compound 5. Compound 5 reacts with thionyl chloride to give compound 6. Compound 6 is then condensed with compounds 7 and 9 to obtain olaparib. This invention uses readily available raw materials, is simple to operate and process, has mild reaction conditions, achieves a total yield of up to 90%, a purity >99%, is environmentally friendly, and is suitable for industrial production.

This invention discloses a synthetic process for an empagliflozin intermediate, belonging to the technical field of pharmaceutical intermediate synthesis. The synthetic process is as follows: 2-chloro-5-bromobenzoic acid is first mixed with dichloromethane and N,N-dimethylformamide, and thionyl chloride is added dropwise to obtain a dichloromethane solution of acyl chloride. Then, it is reacted with fluorobenzene under anhydrous aluminum trichloride catalysis to obtain intermediate EGAB-3. Then, it is dehydrated by azeotropic reaction with potassium hydroxide aqueous solution in toluene, and then refluxed with 3-hydroxytetrahydrofuran under tetrabutylammonium bromide catalysis to obtain intermediate EGAB-7. Then, it is reacted with 1,1,3,3-tetramethyldisiloxane under anhydrous aluminum trichloride and nitrogen protection, dried, and tested to be qualified to obtain empagliflozin intermediate. This process achieves high purity, high yield, and low isomer impurities in the preparation of empagliflozin intermediate.