14 results about "Tosyl chloride" patented technology

The invention discloses a preparation method of tiamulin and tiamulin fumarate based on Bunte salt, which comprises the following steps: mixing the Bunte salt and pleuromutilin p-toluenesulfonate, reacting at 45-65 DEG C for 3-5 hours to synthesize tiamulin, preparing the Bunte salt through a reaction formula 1, and preparing the pleuromutilin p-toluenesulfonate through a reaction formula 2, the molar ratio of the 2-diethylaminoethanol to the sodium thiosulfate to the chlorination reagent in the reaction formula 1 is 1: (1-1.3): (1-1.5), and the molar ratio of the pleuromutilin to the paratoluensulfonyl chloride to the pyridine in the reaction formula 2 is 1: (1-1.2): (1-1.2); the prepared tiamulin and fumaric acid are used as raw materials for a salt forming reaction, the reaction temperature ranges from 55 DEG C to 65 DEG C, the reaction time ranges from 40 min to 80 min, and after the reaction is finished, the tiamulin fumarate is prepared through cooling, crystallization, centrifugation and drying; the tiamulin fumarate disclosed by the invention is high in content, low in total amount of impurities, few in variety and stable in quality under high-temperature and high-humidity conditions, and the preparation method is simple and easy to operate and good in product quality.

The invention discloses a low-damping PVC-U electrical conduit and a processing technology thereof, and belongs to the technical field of conduit preparation. The low-damping PVC-U electrical conduit is prepared from the following components in parts by weight: 70 to 80 parts of PVC resin, 30 to 42 parts of light calcium carbonate, 8 to 15 parts of ethylene-vinyl acetate copolymer, 0.5 to 1 part of ethylene bis stearamide, 3 to 6 parts of epoxy compound and 4 to 7 parts of compound stabilizer, the preparation method comprises the following steps: preparing an epoxy compound from ethyl benzoylacetate, 2-(trimethylsilyl) phenyl trifluoromethane sulfonate, p-toluenesulfonyl azide, p-aminophenol, p-toluenesulfonyl chloride, iodobenzene diacetic acid and rhodium diacetate as raw materials, and preparing the compound stabilizer from 2-(2-aminoethoxy) ethanol, 4-fluorophenol and xylene alkane diisocyanate as raw materials. The PVC-U electrical conduit prepared from the substances has the advantages of low damping, excellent stability, excellent mechanical property and excellent aging resistance.

The present invention provides a quantum dot surface organic ligand composition and a preparation method thereof. The organic ligand composition is synthesized by azeotropic concentration of pentaethylene glycol monoallyl ether and 3-mercaptopropanol under the action of a stabilizer. There are three synthesis methods for pentaethylene glycol monoallyl ether, namely synthesis method 1, synthesis method 2 and synthesis method 3. Among them, synthesis method 1 uses methanesulfonyl chloride and allyloxyethanol as raw materials, reaction formula 2 uses pentaethylene glycol and allyl bromide as raw materials, and reaction formula 3 uses 4-toluenesulfonyl chloride and allyloxyethanol as raw materials. In the process of synthesizing the organic ligand composition of the present invention, a stabilizer is added, which improves the purity stability and viscosity stability of the organic ligand composition, and also greatly improves the binding force and oxidation stability with the quantum dot material. The azeotropic concentration method can remove fine moisture and completely control the gelation phenomenon caused by moisture, and has low viscosity reproducibility.

The present application relates to a kind of continuous synthesis device of p-toluenesulfonyl chloride and synthesis method thereof.The synthesis method described in the present application is as follows:(1) the chlorosulfonic acid of first addition, catalyst, organic solvent are mixed in the first static mixer to obtain mixed liquid A, the mixed liquid A, toluene are pumped into first microreactor respectively to carry out reaction to obtain reaction liquid;(2) the reaction liquid is discharged from the outlet of first microreactor and separates out liquid phase, the liquid phase, the chlorosulfonic acid of second addition are pumped into second microreactor with mixed liquid B in the second static mixer respectively and mixed, carry out reaction in second microreactor to obtain secondary reaction mixture;(3) secondary reaction mixture is discharged from second microreactor and separates out intermediate layer frozen crystallization, filtration, washing, obtains p-toluenesulfonyl chloride.The synthesis method of the present application accurately controls reaction temperature, time, material ratio, greatly improves the production efficiency of p-toluenesulfonyl chloride, green, safe and environmentally friendly.

The present invention discloses a pleuromutilin derivative containing a 2-thio-4-thiazolidinone side chain, and its preparation method and application. The preparation method is as follows: first, pleuromutilin and p-toluenesulfonyl chloride are added to methyl tert-butyl ether, sodium hydroxide solution is added dropwise with stirring, and the reaction is refluxed to obtain intermediate 1; then, 2-thio-4-thiazolidinone is added to acetonitrile, anhydrous potassium carbonate is added and stirred at room temperature for 20 minutes, and then intermediate 1 is added, and the reaction is stirred at room temperature for a certain time to obtain intermediate 2; finally, intermediate 2 and an acyl chloride with different group donors are added to dichloromethane, and under the catalysis of triethylamine, stirred at room temperature for a certain time to obtain a pleuromutilin derivative containing a 2-thio-4-thiazolidinone side chain. The present invention synthesizes a pleuromutilin derivative containing a 2-thio-4-thiazolidinone side chain with good antibacterial activity through a simple preparation process, with high yield, good antibacterial activity against drug-resistant bacteria, and good application prospects.

The present invention discloses a pleuromutilin derivative compound, its preparation method, and application. The method comprises adding pleuromutilin and p-toluenesulfonyl chloride to methyl tert-butyl ether, mixing the mixture, adding sodium hydroxide solution dropwise with stirring, and reacting under reflux to obtain intermediate 1. Intermediate 1 and cysteamine hydrochloride are added to tetrahydrofuran, benzyltributylammonium chloride and sodium hydroxide solution are added dropwise with stirring, and the mixture is reacted with stirring for 4-5 hours to obtain intermediate 2. Intermediate 2, indole acid, and catalyst 2 are added to dichloromethane, and an amidation reaction is carried out at room temperature with stirring for 12-24 hours to obtain the pleuromutilin derivative compound. The pleuromutilin derivative compound of the present invention has a simple preparation process and a high yield. The derivative compound has good in vitro antibacterial activity and is particularly suitable as a new antibacterial drug for preventing and treating infectious diseases caused by bacteria in humans or animals.

Process for preparing the compound of Formula (I) in the form of a base or a salt thereof, said process comprising: a) reacting the compound of Formula (II) with 4-toluenesulfonyl chloride in the presence of a base in an organic solvent, water or a combination thereof, to obtain a compound of Formula (III), b) reacting the compound of Formula (IV) with zinc and iodine in an aprotic polar solvent to obtain a complex between zinc and the compound of Formula (IV); c) reacting the compound of Formula (III) obtained in step a) with the complex zinc-compound of Formula (IV) obtained in step b) in the presence of a catalyst comprising palladium and a phosphine ligand in an aprotic polar solvent to obtain a suspension comprising the compound of Formula (V) d) reacting the compound of Formula (V) in suspension obtained in step c) with a carboxylic acid to obtain a solution of the compound of Formula (VI) e) reacting the compound of Formula (VI) in solution obtained in step d) with an acid having an acid dissociation constant Ka≥1 (also referred to in this text as "strong acid") to obtain the compound of Formula (I).

The invention relates to the technical field of medicine synthesis, in particular to a harmless recycling treatment method for ketoconazole synthesis by-products. The method comprises the following steps: 1, synthesizing ketoconazole by taking cis-bromo-ester, imidazole, potassium carbonate, potassium hydroxide, dichloromethane, ethyl acetate, paratoluensulfonyl chloride, tri-n-propylamine, sodium hydroxide and a ketoconazole side chain as raw materials, and generating wastewater; 2, adding the wastewater in the step 1 into a pH adjusting kettle, adding a proper amount of a pH regulator into the pH adjusting kettle, pumping into a decolorizing kettle, stirring for 1 hour for decolorizing, and pumping into a filter press; step 3, putting the liquid generated in the step 2 into an azeotropic distillation kettle, adding a proper amount of methylbenzene, and heating, refluxing and separating water completely under normal pressure until the water content is less than 0.1%; the byproduct produced in the ketoconazole synthesis process is subjected to innocent treatment, and the production raw materials are recycled, so that the method is energy-saving and environment-friendly, and no waste liquid is discharged.

The application discloses a synthesis method of a high-chirality purity posaconazole mother ring and belongs to the technical field of medicine preparation. In the application, sodium borohydride is used to reduce (R)-3-[(3S,5R)-5-(2,4-difluorobenzene)-5-(iodomethyl)tetrahydrofuran-3-carbonyl]-4-phenyl-2-oxazolidinone containing isomers to an intermediate alcohol, the hydroxyl group of the intermediate alcohol is protected, then the intermediate alcohol is beaten in acetonitrile and filtered to obtain an intermediate; then the intermediate is reacted with sodium triazole to obtain a triazole substituent; finally, the triazole substituent is deprotected into a hydroxyl group, and then p-toluenesulfonyl chloride is added to react, so that the high-chirality posaconazole mother ring is obtained. Compared with the existing preparation technology, the synthesis method provided by the application is simple in operation, high in product yield, low in by-products and high in purity.

The invention discloses a method for synthesizing paratoluensulfonyl isocyanate by a sodium cyanate method. The method comprises the following steps: S1, performing anhydrous treatment on raw materials including sodium cyanate, paratoluensulfonyl chloride and a solvent; s2, adding a certain amount of sodium cyanate, paratoluensulfonyl chloride, a phase transfer catalyst and a solvent into the reaction kettle, and stirring and reacting at 25-30 DEG C for 2-3 hours; s3, filtering out solids from a reaction product in S2, and extracting an organic phase; and S4, distilling the organic phase in S3 to recover the solvent, and performing reduced pressure distillation to obtain p-toluenesulfonyl isocyanate. According to the method for synthesizing the p-toluenesulfonyl isocyanate by the sodium cyanate method, provided by the invention, a high-yield and high-purity product can be obtained by optimizing reaction conditions and purifying steps.

This invention relates to the field of p-toluenesulfonyl chloride production technology, specifically to a hydrolysis apparatus for producing p-toluenesulfonyl chloride. It includes a vessel body, a driving device mounted on the upper end of the vessel body, and a convex box fixed to the outer side of the upper part of the vessel body, communicating with the vessel body. A stirring device is installed inside the vessel body, and the driving device can drive the stirring device to stir the materials inside the vessel body. A pressurizing device is installed inside the convex box, and the movement of a limiting rod can drive the pressurizing device. The pressurizing device is connected to a water tank, and can intermittently pressurize water from the water tank into a connecting hole and an arc-shaped hole, and then spray it out through a nozzle. This invention enables a turntable to drive a rotating ring and a stirring rod to rotate eccentrically inside the vessel body. During the hydrolysis reaction, water can be evenly dripped into the hydrolysis reaction vessel, and stirring can be performed simultaneously during the even dripping of water into the hydrolysis reaction vessel, thereby improving the efficiency of the hydrolysis reaction.

This invention provides a sulfonamide-naphthalimide-TB derivative, its synthesis method, and its application. It is synthesized from p-bromoaniline, paraformaldehyde, p-toluenesulfonyl chloride, ethylenediamine, 4-bromo-1,8-naphthalimide, etc., through a multi-step reaction. Its structural formulas are shown in the first derivative (10) and the second derivative (11) below: The products have large Stokes shifts (both greater than 100 nm) in both solution and solid; they have significant AIE properties; they have a wide pH range and can be applied in the human physiological environment; compared with pure methanol, the fluorescence is enhanced by 1.6 times and 4.3 times at methanol / glycerol = 1 / 9 (v / v), respectively, and both have good responsiveness to viscosity; they can easily enter living A549 cells and have strong targeting ability to their endoplasmic reticulum (Pearson coefficients Pr are 0.81 and 0.71, respectively); the phototoxicity and dark toxicity to A549 cells and HpeG2 cells are both low, indicating that they have high biocompatibility and potential as viscosity probes and endoplasmic reticulum probes for tumor cells.

The invention discloses a ternary positive electrode material of a lithium ion battery, a preparation method of the ternary positive electrode material and the battery. The preparation method comprises the following steps: grinding a hydroxide precursor containing nickel, cobalt and manganese, a lithium salt, nano aluminum oxide and nano cerium oxide into mixed powder; dissolving polyethylene glycol in ethanol, adding paratoluensulfonyl chloride for reaction, extracting reaction liquid, and drying an oily organic phase; trimethyl phosphite is added into the organic oil phase, washing and drying are performed after heating reaction, then the organic oil phase is added into concentrated hydrochloric acid for hydrolysis, and a surfactant is obtained; and adding the mixed powder into a surfactant, treating, and calcining at high temperature to obtain the ternary positive electrode material of the lithium ion battery, according to the invention, the surfactant is used for assisting in synthesis of the single-crystal ternary positive electrode material, and single-crystal particles with good dispersibility and uniform particle size are obtained; and the surface active agent is used for regulating and controlling the crystal face exposure and the particle shape of the single crystal particles, so that the lithium ion diffusion rate is improved, the lithium ion transmission dynamics is improved, and the electrode material has relatively high specific capacity and relatively long cycle life.

The invention relates to the technical field of synthetic chemistry, in particular to a method for preparing 4-bromo-3-methoxyphenol. Comprising the following steps: (1) hydrolyzing a compound of formula I to generate a compound II; (2) reacting the compound shown in the formula II with toluene-4-sulfonyl chloride to generate a compound III; (3) reducing the compound in the formula III to generate a compound IV; (4) reacting the compound shown in the formula IV with nitrite or nitrite ester, and then reacting with a bromination reagent to generate a compound V; and (5) hydrolyzing the compound of formula V to generate a compound VI. According to the preparation method provided by the invention, the target product 4-bromo-3-methoxyphenol is efficiently prepared under mild conditions through the reaction steps of hydrolysis, substitution, reduction, bromination and the like, so that the problems of harsh oxidation reaction conditions, no reaction selectivity concern and high total molar yield of the original process are avoided, and the preparation method has the advantages of more controllable quality, high atom economy, low cost and the like. The process is stable, and production is easy. The synthesis route is shown in the specification.