113 results about "Dithiete" patented technology

The invention discloses a high-selectivity beta-triazole (beta-triazole trifluoromethyl, beta-triazole ketone, beta-triazole sulfo and beta-triazole seleno) derivative as well as a synthesis method and application thereof.The high-selectivity beta-triazole (beta-triazole trifluoromethyl, beta-triazole ketone, beta-triazole sulfo and beta-triazole seleno) derivative is prepared from a triazole compound, an alkyl compound / aldehyde / disulfide / diselenide and styrene as raw materials in an oxidizing agent, an additive and an organic solvent in a one-pot reaction mode, and the high-selectivity beta-triazole (beta-triazole trifluoromethyl, beta-triazole ketone, beta-triazole sulfo and beta-triazole seleno) derivative is obtained. The product can be obtained with high selectivity and high yield through one-step reaction. The method provided by the invention has the advantages of good selectivity, mild reaction conditions, high yield, simple and safe operation, high efficiency and the like. The beta-triazolone derivative compound provided by the invention is of a brand new structure and has good anti-osteosarcoma activity, and biological activity analysis shows that part of the compound can achieve 99% inhibition rate on osteosarcoma (OS) cell lines 143B, MNG / HOS and SJSA-1 under the concentration of 10 [mu] M. Therefore, the compound can be used as an important intermediate of medicine and chemical industry, and has a wide application prospect in the field of medicine.

The invention discloses a method for determining the content of bis (2-aminophenyl) disulfide in 2-aminothiophenol. The method comprises the following steps: preparing an acetonitrile solution of citric acid as a diluent; preparing a system applicability solution, a reference solution and a test solution by using a diluent; a diluent, a system applicability solution, a reference substance solution and a test solution are sequentially injected by adopting a liquid chromatography, and the content of bis (2-aminophenyl) disulfide in a 2-aminothiophenol sample is determined by adopting an external standard method. The antioxidant citric acid is added into the diluent, so that the generation of the disulfide compound is inhibited, the existing disulfide compound is not damaged, the solution stability is high, the operation is simple, the system applicability, specificity, accuracy, precision and durability completely accord with the guidance principle verified by the Chinese pharmacopoeia method, and the method is suitable for industrial production. The method can be used for quality control of 2-aminothiophenol.

The invention relates to the technical field of preparation of compounds, in particular to a sulfenamide compound and a preparation method thereof. Compared with the prior art, a mild electrochemical method is adopted for preparing the sulfenamide compound forming the N-S bond, in the reaction process, halide salt serving as electrolyte is subjected to oxidation reaction at an anode to obtain free radicals, and after decarburization of an amine compound is promoted by the free radicals and alkali together, the free radicals react with disulfide or mercaptan to form the sulfenamide compound forming the N-S bond; the method disclosed by the invention has the advantages of good substrate compatibility and functional group tolerance, no need of additional addition of an oxidizing agent and a transition metal catalyst, simple reaction post-treatment operation and the like, is convenient to operate, high in atom utilization rate and mild in reaction condition, meets related requirements of green chemistry, and has a good development prospect.

The invention belongs to the technical field of polyurethane, and provides a railway polyurethane elastic backing plate with a self-repairing function and a preparation method thereof.The railway polyurethane elastic backing plate is prepared from, by mass, 60-80 parts of isocyanate prepolymer, 14-16 parts of cross-linking agent, 4-6 parts of chain extender and 0.6-0.8 part of catalyst; the cross-linking agent comprises a cross-linking agent A and a cross-linking agent B in a mass ratio of 1: (0.5-1); wherein a preparation method of the cross-linking agent A comprises the following steps: stirring and reacting diphenylmethane diisocyanate and 4, 4 '-diaminodiphenyl disulfide in a mass ratio of 2: 1 at 60-65 DEG C in the presence of a catalyst for 2-3 hours; a preparation method of the cross-linking agent B comprises the following steps: stirring and reacting diphenylmethane diisocyanate and 2, 2 '-diaminodiphenyl disulfide in a mass ratio of 2: 1 at 85-90 DEG C in the presence of a catalyst for 2-3 hours. By introducing disulfide bonds, the self-repairing function is achieved, and the service life of the elastic base plate is prolonged; meanwhile, due to the good mechanical property and stability, the composite material can be normally used in various severe environments and has a wide application prospect.

The invention belongs to the technical field of organic synthesis, and discloses a synthesis method of a disulfide compound. According to the invention, under the catalytic action of 1, 4, 7, 10, 13, 16-hexaoxacyclo-octadecane, halogenated hydrocarbon, sodium sulfide and sulfur react at the temperature of 50-60 DEG C to prepare the disulfide compound. The synthesis method of the disulfide compound has the advantages of being simple in process, small in catalyst dosage, mild in reaction condition, high in production efficiency, low in production cost, convenient for industrial production and the like, in addition, the reaction yield of the synthesis method can reach 94.8%-96.6%, and the purity of the obtained target product reaches up to 97.9%-99.3%. The method can be applied to preparation of the disulfide compound, and the obtained disulfide compound can be further applied to the fields of biomedicine, agriculture, chemical industry and the like.

The invention discloses high-toughness self-repairing polyurethane based on a ureido / disulfide bond dual dynamic network and a preparation method of the high-toughness self-repairing polyurethane, and belongs to the technical field of self-repairing high polymer materials. The structural formula of the thermal stimulation repairing polyurethane is shown in the specification. The polyurethane is formed by mixing and polycondensing polyether amine, diaminodiphenyl disulfide and dicyclohexylmethane diisocyanate. According to the invention, polyether amine is used as a raw material, green synthesis without a catalyst is realized, ureido generated by the reaction forms a hydrogen bond network with extremely strong dynamic property and cooperates with a disulfide bond, a repair process is completed at 50 DEG C, the toughness can reach 40.55 MJ / m < 3 >, the fast recovery capability is realized, the material can be stretched to be 20 times of the original length, and the service life of the material is prolonged. Good network dynamic property is achieved at the room temperature, and high self-repairing efficiency is achieved at the room temperature.

The invention discloses a compound cis-3-hexenyl disulfide. The specific chemical structural formula of the compound cis-3-hexenyl disulfide is as follows: # imgabs0 #. The aromatic compound is mainly applied to food essence.

The invention belongs to the technical field of organic synthesis, and provides a preparation method of diphenyl disulfide, which comprises the following steps: A, in a dry atmosphere filled with inert gas, mixing halogenated benzene and magnesium powder, reacting to generate a Grignard reagent, and cooling to 0-15 DEG C; and B, dissolving disulfur dichloride in a solvent, dropwise adding the solution into the Grignard reagent obtained in the step A, carrying out a stirring reaction at 0-15 DEG C, carrying out a quenching reaction by using a saturated ammonium chloride aqueous solution, and carrying out extraction, drying and concentration on an organic phase to obtain diphenyl disulfide. The method adopts a one-pot method for direct synthesis, and is green and environment-friendly, and high in yield and purity.

The invention belongs to the technical field of organic synthesis, and discloses a symmetric disulfide compound containing a sulfoxide group and application of the symmetric disulfide compound in glycosylation reaction, and the structural general formula of the compound is as shown in formula (I). According to the present invention, the compound represented by the structural general formula (I) contains sulfoxide and disulfide structures, and the sulfinyl forming the sulfoxide and the disulfide bond-containing group are located at the ortho-position of the aromatic ring, such that the compound can be used as the activation reagent for the glycosylation reaction, and particularly, activation of the glycosyl donor and glycosylation reaction can be efficiently promoted by only using 0.25 times of equivalent weight of the glycosyl donor, so that the use of a highly toxic, expensive, unstable or metal-containing activating reagent is avoided, and the problems that the activating reagent of the thioglycoside donor in the existing glycosylation reaction is unstable, is not easy to prepare and often needs equivalent weight or excessive amount are solved.

The present disclosure relates to a method for oxidation of mercaptans, comprising the following steps: contacting mercaptan compounds with a catalyst for oxidation reaction in the presence of oxygen; the catalyst is a composite catalytic material, which comprises a full-silica molecular sieve and a metal element M dispersed in the intracrystalline of the full-silica molecular sieve; the metal M is selected from one or more of manganese, iron, cobalt, nickel, palladium, platinum, copper and gold. The present disclosure uses a metal-containing hierarchical porous molecular sieve for mercaptan oxidation and dehydrogenation reaction, without adding additional alkali, high conversion rate and disulfide selectivity can be obtained at a lower temperature, which has high industrial application value.

The invention discloses a preparation method of a high-adhesion self-repairing polyurethane elastomer, which specifically comprises the following steps: taking polytetrahydrofuran glycol and isophorone diisocyanate as raw materials, taking tannic acid and 4, 4 '-diaminodiphenyl disulfide as chain extenders, and adopting a one-pot polymerization method to prepare high-adhesion polyurethane. The polyurethane elastomer is endowed with self-repairing performance by introducing an aromatic group disulfide bond and a dynamic hydrogen bond, the prepared material can complete the repairing process within 2 hours at the temperature of 80 DEG C, and the adhesive force on steel is greater than 10 MPa. A new insight is given to preparation of a high-adhesion self-repairing material, the synthesis method is simple, and the prepared polyurethane has excellent adhesion and self-repairing performance and can be applied to multiple fields.

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of a thiohydrazone compound. The synthesis method of the thiohydrazone compound comprises the following steps: taking (isocyano-imino) triphenylphosphine and one of thiophenol substances, thiol substances and disulfide substances as reactants, taking methanol or a mixed solution of methanol and water as a solvent, carrying out a reaction, and carrying out separation and purification to obtain the thiohydrazone compound. The synthesis method provided by the invention has the advantages of mild conditions, no need of additional metals and additives, easy separation of products, high yield and green and efficient reaction.

This invention relates to a non-natural methionine and its synthesis method, using inexpensive and readily available transition metals as catalysts. N Using arylglycine, styrene compounds, and disulfides as raw materials, a series of non-natural methionine compounds were obtained with high selectivity and high yield through a three-component reaction under mild conditions. The compounds prepared in this invention are multifunctional non-natural methionine derivatives, representing a novel class of natural methionine derivatives. They can be used in drug modification, biosensor fabrication, and other fields, possessing significant research and application value and providing new synthetic strategies for the preparation of novel peptide drugs.

The invention discloses a preparation method of bis (2, 3-epithiopropyl) disulfide, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: reacting epichlorohydrin with thioacetate to obtain 2-(acetylthiomethyl) ethylene oxide; then reacting with hydrochloric acid for deacetylation protection; reacting with hydrogen peroxide under the catalysis of iodine, or reacting with sulfur powder and sodium hydroxide; and finally, reacting with thiourea to obtain the bis (2, 3-epithiopropyl) disulfide. The chloropropylene oxide is used as the raw material, the intermediate in the whole reaction process can be purified, the final product is high in purity, and the obtained product can be used for high-refractive-index resin lenses (the refractive index is larger than or equal to 1.70) and high-temperature-resistant optical coatings and meets the requirements of the electronic and medical fields.

The invention discloses a preparation method of bis (2, 3-epithiopropyl) disulfide, which comprises the following steps: step 1, dissolving epichlorohydrin in a solvent, adding a catalyst A, and introducing a vulcanizing agent A for reaction; step 2, adding a catalyst B into a system in the step 1, stirring and dissolving, then adding an oxidant, and controlling the temperature to carry out oxidation reaction; 3, after the reaction is finished, cooling, adding an organic solvent, dropwise adding an alkaline reagent, continuing the reaction, after the reaction is finished, standing for layering, separating out an organic layer, and washing with water; and step 4, supplementing the same amount of organic solvent into the organic layer obtained in the step 3, adding a vulcanizing agent B under the protection of inert gas, carrying out temperature control reaction, washing the reaction liquid after the reaction is finished, and carrying out rotary evaporation to remove the solvent to obtain a finished product. The temperature is controllable, high-temperature and high-pressure conditions do not exist, the purity of the obtained product is high, and industrial production is facilitated.

The present invention belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing thiosemicarbazone compounds. The method for synthesizing thiosemicarbazone compounds uses (isocyanimino) triphenylphosphine and one of thiophenol substances, thiol substances, and disulfide substances as reactants, and uses methanol or a mixed solution of methanol and water as a solvent for reaction. After separation and purification, thiosemicarbazone compounds are obtained. The synthesis method of the present invention has mild conditions, does not require additional metals and additives, the product is easy to separate and has a high yield, and the reaction is green and efficient.

The invention belongs to the field of organic synthesis, and relates to a method for constructing S-glucoside through visible light catalysis of a sugar molecule deoxidation vulcanization reaction. Mixing a carbohydrate compound, an additive, first alkali and a first solvent to obtain a first mixed solution; uniformly mixing a disulfide compound, a photocatalyst, second alkali and a second solvent to obtain a second mixed solution; and mixing the first mixed solution with the second mixed solution, and carrying out a photoreaction under visible light to obtain the thioether compound containing S-glucoside. Through an NHC-photooxidation reduction synergistic mechanism, the reaction can be efficiently completed within 2 hours, the yield can reach 26%-67%, the reaction efficiency and the operation safety are remarkably improved, and meanwhile, the problems of energy consumption and metal catalyst residues are reduced.

The present invention belongs to the field of preparation methods of aliphatic disulfides, and particularly relates to a method for catalytic synthesis of symmetrical dialkyl disulfides, which is implemented according to the following steps: (1) Place a magnetic stirrer bar, measured thiol, sulfur, and an organic superbase catalyst into a reaction flask; (2) Place the reaction flask in an oil bath of a magnetic heating stirrer, install a condenser, and connect the condenser to a drainage bottle through a silicone rubber tube. A saturated aqueous solution of H<subgt;2< / subgt;S is pre-added to the drainage bottle; (3) Start heating and begin stirring the reaction, start timing, and determine the amount of H<subgt;2< / subgt;S released and the reaction termination time by the drainage method to obtain the target product. The reaction conditions of the present invention are mild, the reaction rate is fast, the atomic utilization rate and the yield are high, and the by-product H<subgt;2< / subgt;S gas is easily separated and utilized.

The invention provides size-controllable palladium nanoparticles as well as a preparation method and application thereof. The preparation method of the size-controllable palladium nanoparticles comprises the following steps: fully dispersing potassium tetrachloropalladate, tris (4-fluorophenyl) phosphine, 4, 4-dichlorodiphenyl disulfide, sodium salt and a reducing agent in a solvent, reacting, filtering, washing and drying to obtain the size-controllable palladium nanoparticles, the sodium salt is sodium hexafluoroantimonate or sodium tetrafluoroborate. According to the invention, a plurality of palladium nanoparticles with stable ligands (phosphine, mercaptan and anions) are systematically designed and synthesized, the preparation method is simple, and the reaction conditions are easy to realize; by changing the anion ligand SbF6 <-> or BF4 <->, the palladium nanoparticles with different sizes are obtained at a good yield. The palladium nanoparticles are applied to catalysis of the reduction reaction of 4-nitrophenol, and an excellent catalytic effect is shown.

The invention discloses a synthesis process of high-yield sodium benzenesulfinate, and belongs to the technical field of synthesis of sodium benzenesulfinate. The synthesis process of the high-yield sodium benzenesulfinate comprises the following preparation steps: S1, mixing a first catalyst, sodium hydroxide and a first solvent, then adding powdered sulfur, reacting for a first reaction time under microwave radiation, then adding chlorobenzene, continuously reacting for a second reaction time under microwave radiation, then filtering, carrying out reduced pressure distillation to remove the solvent, and recrystallizing, so as to obtain the high-yield sodium benzenesulfinate. The diphenyl disulfide is obtained; s2, mixing the diphenyl disulfide prepared in the step S1, alcohol, an oxidizing agent and a second solvent, stirring in the air at room temperature for a third reaction time, diluting with ultrapure water, extracting with ethyl acetate for multiple times, combining organic layers, drying, concentrating and purifying to obtain benzene sulfinate, and keeping in a dark place and in an oxygen-isolated manner; s3, under the dark and nitrogen conditions, benzene sulfinate prepared in the step S2 is hydrolyzed and refined under the alkaline condition, and sodium benzene sulfinate is obtained.

The invention provides application of a dialkyl disulfide compound as a collecting agent in copper-molybdenum bulk flotation, the general formula of the dialkyl disulfide compound is R1-S-S-R2, R1 and R2 are respectively and independently at least one of C1-C12 alkyl and C1-C12 alkenyl, and R1 and R2 are respectively and independently at least one of C1-C12 alkyl and C1-C12 alkenyl. According to the method, the dialkyl disulfide compound serves as the collecting agent to be applied to copper-molybdenum bulk flotation, the recovery rate of copper and molybdenum in minerals can be effectively increased, and loss of valuable metal in tailings is reduced.

This invention relates to a method for synthesizing aromatic carbon-10 sulfur-containing compounds from isoprene. Specifically, using disulfide, isoprene, and 2-methyl-1-buten-3-yne as raw materials, aromatic carbon-10 sulfur-containing compounds are constructed under cobalt catalyst and iodine tandem catalysis. This invention has the following advantages: the raw materials are simple and readily available, the synthesis is simple, it is environmentally friendly, the conditions are mild, and it has high atom economy. The compounds obtained from the bulk chemical isoprene have structures similar to natural terpenes and represent an important class of terpenes.

The present invention relates to the technical field of composite films, specifically a low-reflection explosion-proof multi-layer composite film and its preparation process, which comprises a base film, an antireflection layer, and a protective layer laminated in sequence. A self-healing prepolymer, amino-functionalized composite zinc oxide, a leveling agent, and a dialdehyde-based ionic liquid are introduced to construct a low-reflection explosion-proof multi-layer composite film with a self-healing antibacterial superhydrophobic surface; an amino-terminated polydimethylsiloxane reacts with diphenylmethane diisocyanate and isophorone diisocyanate to prepare a prepolymer containing silicone, and then diaminodiphenyl disulfide is used as a chain extender, and polyether triol and perfluorooctylethanol are used as end-capping agents; titanium dioxide is first synthesized on the surface of zinc oxide, and using the hydroxyl groups on its surface, asparagine is used as a raw material to obtain amino-functionalized composite zinc oxide; a dialdehyde-based ionic liquid is introduced into the protective layer.

A novel disulfide biphenol ether compound and its preparation method and application for treating inflammatory skin diseases, the structural formula of the disulfide biphenol ether compound is: biphenyl diester is first dissolved in anhydrous tetrahydrofuran solvent, lithium aluminum hydroxide is added, quenched, filtered, extracted with dichloromethane, water is added to quench the reaction, extracted with dichloromethane, the organic phases are combined, after removing residual moisture, the reduced pressure rotary evaporation and recrystallization are removed to obtain intermediate 2; intermediate 2 and potassium thioacetate are added to solvent N, N-dimethylformamide and extracted, the organic phases are combined, and the solvent is evaporated and concentrated to obtain a light intermediate 3; intermediate 3 is dissolved in anhydrous methanol, sodium methoxide is added, stirred, extracted with ethyl acetate, and the organic phases are combined to obtain. The disulfide biphenyl compound prepared by the present invention has good anti-inflammatory ability, can effectively reduce inflammatory infiltration in tissue, improve the inflammatory phenotype of animal models, and can prevent and treat inflammatory skin diseases.

The invention discloses a Karl Fischer moisture determination method for sulfur-containing organic compounds, and belongs to the technical field of chemical analysis. The method comprises the following steps: adding absolute methanol, imidazole and an inhibitor (selected from N-substituted maleimide or acrylate compounds) into a titration system, then adding a sample, and titrating with a pyridine-containing Karl-Fischer reagent to the end point. The inhibitor can effectively capture reducing sulfur species and eliminate interference of the reducing sulfur species on iodine. Experiments show that for sulfur-containing samples such as 2, 2-dimethylthiopropane, dimethyl sulfide, dimethyl disulfide and the like, the deviation reduction rate of the method is more than 60% compared with that of a traditional method; the method is easy and convenient to operate, high in accuracy and suitable for moisture analysis of sulfur-containing organic matter in the fields of petrifaction, pharmacy and the like.

The application discloses a kind of high selectivity β-triazole (β-triazole trifluoromethyl, β-triazole ketone, β-triazole thio, β-triazole selenide) Derivative and its synthesis method and application, with triazole compound, alkyl compound / aldehyde / dithioether / diselenide and styrene as raw material, in oxidant, additive and organic solvent, through one step reaction can high selectivity, high yield product is obtained.The method of the application has the advantages of good selectivity, mild reaction condition, high yield, simple and safe operation and high efficiency etc.The β-triazole ketone derivative compound involved in the application is a kind of new structure, has good anti-osteosarcoma activity, biological activity analysis shows that part of compounds can reach 99% inhibition rate to osteosarcoma (OS) cell line 143B, MNG / HOS and SJSA-1 at 10 μM concentration.Therefore, the compound can be used as important pharmaceutical and chemical intermediates, and has wide application prospect in the field of medicine.

The application belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing 1-(2,4-dimethylphenyl)thio-N-benzyl-2-naphthylamine by a continuous flow light-heat integrated method. The method is performed in a micro-channel reaction device provided with light and heat. N-benzyl-2-naphthylamine, 2,2',4,4'-tetramethyl diphenyl disulfide and a catalyst sodium iodide are dissolved in acetonitrile solvent to obtain a reaction solution. A blue light is used as a light source of a reaction module, and the temperature is adjusted to 25-60 DEG C. Air or oxygen is introduced into the reaction solution, and magnetic stirring is performed. Then, the gas-liquid mixed reaction solution is input into the reaction module through a peristaltic pump to obtain 1-(2,4-dimethylphenyl)thio-N-benzyl-2-naphthylamine. The application creatively uses the continuous flow light-heat integrated reaction technology to synthesize 1-(2,4-dimethylphenyl)thio-N-benzyl-2-naphthylamine, greatly improves the reaction efficiency, shortens the reaction time, improves the safety and controllability of the reaction, solves the amplification effect of the conventional reaction, and provides a reaction technology without bottleneck amplification for the synthesis of the compound.

The invention belongs to the field of catalytic organic synthesis and relates to a green preparation method of diphenyl sulfide and its derivatives. The invention first uses zeolite molecular sieve to load metallic iron to prepare a catalyst in which divalent Fe and trivalent Fe coexist, namely, Fe(II) / Fe(III)-ZSM-5 catalyst, and then uses the catalyst in the desulfurization reaction of diphenyl disulfide and its derivatives, wherein the ZSM-5 zeolite carrier plays a role in activating Fe atoms and reactants, and the iron atoms have catalytic oxidation properties on the surface of the zeolite, and can efficiently and greenly realize the reaction in a heterogeneous phase, without the participation of halogenated substances and without the participation of ligands, so as to prepare diphenyl sulfide and its derivatives, increase the atomic economy of the synthesis process, reduce the separation difficulty of the system, and finally obtain a catalyst that can achieve a very high conversion rate and excellent product selectivity under the catalytic conditions of using air and oxygen as oxidants and without the participation of ligands.

The invention provides a method for synthesizing a series of polyfluoroalkyl 1, 2-alkene disulfide compounds by performing dehalogenation 1, 2-double vulcanization reaction on polyfluoroalkyl olefin and a disulfide compound under the promotion of sodium hydroxide under a metal-free condition. The reaction conditions are mild, the tolerance of functional groups is good, the method has the characteristics of simple post-treatment, green steps, low pollution, high economic benefits and the like, and part of the polyfluoroalkyl 1, 2-ene disulfide compounds show certain activity of inhibiting human colon cancer cells (HT-29) and are used for preparing the human colon cancer cell activity inhibitor.

The invention discloses a remodelable and degradable bismaleimide resin and a preparation method thereof, which is prepared by 4,4'-dithiodiphenylamine bismaleimide (AM), 4,4'-diallyloxydiphenyl disulfide (DS) and phenolphthalein polyaryletherketone. The bismaleimide resin prepared by the invention not only has excellent heat resistance, but also can be remodeled under hot pressing conditions; it can achieve faster degradation in conventional solvents, and the degradation solution can be evaporated of the solvent, heated and pressurized to achieve closed-loop recovery, which overcomes the shortcomings of bismaleimide resins containing reversible covalent bonds that are difficult to have high heat resistance, remodelability and degradability, and provides new resins and preparation strategies for achieving sustainable development of heat-resistant thermosetting resins.