198 results about "Sulfohydrazide" patented technology

The invention provides a method for preparing sludge-based formed magnetic active carbon. The method comprises the steps as follows: sludge is used as a raw material, an activating agent is added for carbonizing and activating the sludge; nano-sized Fe3O4 is used as a magnetic source for magnetizing the sludge active carbon; and sodium carboxymethylcellulose and aluminum salt are composited to an organic-inorganic binding agent, the binding agent and a p-toluenesulfonhydrazide foaming agent are used for uniformly binding powdery magnetic active carbon into a formed magnetic active carbon precursor with abundant pore structures, and finally, the formed magnetic active carbon precursor is heated to obtain the sludge-based formed magnetic active carbon. According to the method, the sludge is used as a main raw material, the resource utilization of the sludge is achieved, the recycling is convenient, and reutilization can be achieved; and further, the sludge-based formed magnetic active carbon has a stable structure and good magnetic stability, and can be widely used in the fields such as sewage treatment, soil pollution treatment and the like.

The invention discloses an electrochemical catalysis synthesis method of a 3-sulfonyl substituted oxo indoles compound, and belongs to synthesis of compounds. The method uses a sulfoacid reagent represented by a formula (III) or sulfonyl hydrazine represented by a formula (V) or N-substituted acrylamide represented by a formula (II) as a raw material in a single-cell electrolytic tank; and in presence of an electrocatalyst, the raw material is electrolyzed in electrolyte at a certain temperature to obtain the 3-sulfonyl substituted oxo indoles compound represented by a formula (I). The method firstly adopts an operation-simple electrochemical catalysis indirect electrolysis method to synthesize the 3-sulfonyl substituted oxo indoles compound, uses the single-cell electrolytic tank and constant-current electrolysis, uses a cheap and easy-obtained graphite piece as a working electrode, largely reduces the cost, in particular, reduces heavy metal or chemical-metered oxidant, prevents generation of chemical wastes, is simpler in operation, and is more suitable for industrial production.

The invention discloses a method for synthesizing 2-sulfonyl ketone compounds. The method comprises the following steps: mixing substituted N-vinyl acetamide, sulfohydrazide compounds, a catalyst, an oxidant and a solvent to obtain a mixed liquid; and reacting for 2-12 hours at 20-120 DEG C; and then, decompressing to remove the solvent and separating to obtain the 2-sulfonyl ketone compounds, wherein the catalyst is organic amine salt, the oxidant is peroxide and the molar ratio of the sulfohydrazide compound to the substituted N-vinyl acetamide is (1-3):1. The invention provides a new route for synthesizing the 2-sulfonyl ketone compounds. By taking N-vinyl acetamide and the sulfohydrazide compounds as raw materials, the substrate is good in adaptability and corresponding 2-sulfonyl ketone compounds can be synthesized by various substituents. The method is mild in reaction condition, safe and environmental friendly and free from exhaust gases.

The invention relates to a preparation method of a sulfuryl fluoride compound. A sulfonyl hydrazide compound and a fluoride reagent serve as reaction raw materials. The preparation method includes the steps that a, the sulfonyl hydrazide compound with the structure (I) and the fluoride reagent are dispersed in a solvent, wherein the structure (I) is shown in the specification; b; a mixture obtained from the step a is stirred and heated to obtain the sulfuryl fluoride compound with the structure (II), wherein the structure (II) is shown in the specification (II). Compared with existing related technologies in the chemical synthesis field, the method of preparing sulfuryl fluoride from sulfonyl hydrazide is achieved for the first time. In the method, no catalyst needs to be added, reaction conditions are moderate, good compatibility can be achieved for water and air, and large-scale production is easy to achieve. The experimental result indicates that the yield of the obtained sulfuryl fluoride compound can reach up to 98%.

The invention provides a preparation method for alpha-iodo-beta-arylketo-substituted sulfone compounds. The preparation method comprises the following steps: taking olefin nitrine, sulfohydrazide and potassium iodide as starting raw materials; and in an organic solvent, taking tert-butyl hydroperoxide as an oxidizing agent, and reacting to generate the alpha-iodo-beta-arylketo-substituted sulfone compounds, wherein a molar ratio of olefin nitrine to sulfohydrazide to potassium iodide to tert-butyl hydroperoxide is 1:2:2:2, the reaction temperature is the room temperature, and the reaction time is 2-4 hours. The preparation method provided by the invention is reasonable in design, adopts easily available raw materials, does not need a metal catalyst, is gentle in reaction condition, is free of high-temperature flux, is safe and convenient and is high in yield, and the yield of most products is 70% or higher, so that the preparation method is a method, which is simple to operate, quick, gentle and diversified, for constructing the alpha-iodo-beta-arylketo-substituted sulfone compounds, wherein the three starting raw materials can be obtained through a one-step process, and the reaction raw materials are cheap and easily available; and the formulas of the alpha-iodo-beta-arylketo-substituted sulfone compounds are as shown in the specification.

The invention relates to a preparation method of ivermectin. The ivermectin is prepared by taking an abamectin B2 component as a raw material and removing 23-position sulfonyl hydrazone of the abamectin B2 through reduction, and the process comprises the following steps: (1) protecting 4''-position hydroxyl and 5-position hydroxyl of the abamectin B2 with allyl carbonate; (2) oxidizing 23-position hydroxyl of the abamectin B2 into keto carbonyl; (3) converting the 23-position keto carbonyl of the abamectin B2 with organic sulfonyl hydrazine into hydrazone, thus generating the 23-position sulfonyl hydrazone of the abamectin B2; and (4) reducing with hydroborate to remove the 23-position sulfonyl hydrazone of the abamectin B2, and simultaneously removing the 4''-position protecting group and the 5-position protecting group to obtain the ivermectin. The total yield of the reaction is up to 67-72%. According to the invention, the ivermectin is prepared by taking the abamectin B2 component as the raw material, the utilization range of the abamectin B2 is widened, the cost of the ivermectin is reduced, the preparation conditions are mild, the yield is high, and the use of virulent tributyltin hydride Bu3SnH is avoided. Thus, the invention is suitable for industrial production.

The invention relates to piperine hydrazone, acylhydrazone or sulfonyl hydrazone derivative substances and application for preparing a botanical insecticide. The piperine hydrazone, acylhydrazone or sulfonyl hydrazone derivative substance takes the piperine hydrazone as raw materials, piperine aldehyde is obtained by means of hydrolysis, esterification, reduction and oxidation, and the piperine aldehyde is respectively reacted with replaced phenylhydrazine, the acylhydrazone and sulfonyl hydrazide. The structural formula is shown as follows. The experiment shows that the piperine hydrazone, or the acylhydrazone or the sulfonyl hydrazone derivative substances has the advantages of having good antifeedant and insecticidal activity, partly exceeds the parent piperine, wherein the insecticidal activity of some components is higher than the commercialized botanical pesticide toosendanin, and therefore the piperine hydrazone, or the acylhydrazone or the sulfonyl hydrazone derivative substances is expected to be used for preparing high-efficient, environment-friendly and low-toxic botanical insecticides.

The invention relates to a synthetic method of a marine terpenoid natural product namely ent-chromazonarol, and belongs to the field of chemical synthesis. The synthetic method provided by the invention uses salvia sclarea aldehyde and 2-iodo-1,4-dimethoxybenzene as starting materials. Salvia sclarea sulfonyl hydrazone is generated by a condensation reaction between salvia sclarea aldehyde and p-toluenesulfonyl hydrazide, an olefinic alcohol compound is obtained by a coupling reaction between salvia sclarea sulfonyl hydrazone and 2-iodo-1,4-dimethoxybenzene, an olefinic terpene compound is obtained by an intra-molecular reductive reaction and a double-bond isomerization reaction of the olefin alcohol compound, an olefinic phenol compound is obtained by an oxidation reaction and a reduction reaction of the olefinic terpene compound, and a target marine terpenoid natural product namely ent-chromazonarol is obtained by a cyclization reaction of the olefinic phenol compound. The synthetic method provided by the invention has the characteristics of few reaction steps, simple and convenient operation, good product selectivity, suitability of industrial production, and the like.

The invention discloses a preparation method of a white carbon black high-activity dispersing agent composition. The preparation method comprises the following steps: weighing the following materials in percentages by weight: 20%-60% of at least one of hydrazide and sulfohydrazide, 25%-50% of long-chain fatty acid, 1%-15% of octadecanol, 1%-15% of diethylene glycol, 1%-15% of monoglyceride, 1%-20% of hexadecyl trimethyl ammonium chloride and 1%-20% of C9 resin; putting the long-chain fatty acid, octadecanol, diethylene glycol, monoglyceride, hexadecyl trimethyl ammonium chloride and the C9 resin into a negative-pressure reaction kettle; increasing the temperature; adding at least one of hydrazide and sulfohydrazide into the reaction kettle, thus obtaining the white carbon black high-activity dispersing agent composition after the reaction is finished. The preparation method is simple in technology and easy to operate; in a formula of rubber filled with white carbon black, the added composition is capable of increasing the activity of the white carbon back and improving the dispersing effect of the white carbon back in the rubber, and then enhancing the physical mechanical property of vulcanized rubber.

The invention discloses a light sensitization composition using a sulfonyl hydrazone compound. The composition comprises a dissolving resistant/dissolving promotion agent, an alkali soluble line type phenolic resin, an infrared absorption dye, a background dye and a solvent, wherein the dissolving resistant/dissolving promotion agent is a cyclohexanone sulfonyl hydrazone compound. The sulfonyl hydrazone compound provided by the invention is added into the light sensitization composition and can be quickly subjected to chemolysis to generate N2 for foaming only when the temperature of a scanning area is higher than 170 DEG C. In the decomposition foaming process, the membranous layer of the scanning area is loosened and is easy to develop, and most of small segments remained on the membranous layer after the decomposition are acidic materials of different types, so that an obvious dissolving promotion effect is generated during alkali development, and the composition has high thermal stability and long service life. Therefore, the cyclohexanone sulfonyl hydrazone compound is used as the dissolving resistant/dissolving promotion agent of the light sensitization composition, so that a thermosensitive computer to plate (CTP) board with high sensitivity and high development speed can be obtained.

The invention relates to a synthesis method of a marine natural product Puupehedione, and belongs to the field of chemical synthesis. (-)salvia sclarea aldehyde and 1-iodine-2,4,5-trialkoxy benzene are used as starting materials, (-)salvia sclarea aldehyde and p-toluenesulfonhydrazide generate salvia sclarea hydrazone 2, salvia sclarea hydrazone 2 and 1-iodine-2,4,5-trialkoxy benzene form a framework compound 4 of Puupehedione under the catalysis of palladium in a coupling manner, the framework compound 4 is oxidized into an intermediate quinine under the action of an oxidizing agent, and quinine and C-8 site hydroxyl are subjected to reaction, so as to realize cyclization, isomerization and dealcoholization reactions to obtain natural product Puupehedione in one step. The synthesis method has the characteristics of being few in reaction steps, simple and convenient to operate, good in product selectivity and suitable for industrial production.

The invention discloses a synthetic method of (E)-alkenyl sulfone compounds. The method comprises the following steps: beta-nitroolefin compounds shown as formula I in the description, sulfohydrazidecompounds shown as formula II in the description, an iodine-containing nonmetal catalyst and a peroxide oxidizing agent are mixed for a reaction, and a mixture obtained after the reaction is subjectedto postprocessing, and the (E)-alkenyl sulfone compounds shown as formula III in the description are obtained. Beta-nitroolefin compounds, the sulfohydrazide compounds, the iodine-containing nonmetalcatalyst and the peroxide oxidizing agent are taken as main raw materials, the corresponding (E)-alkenyl sulfone compounds are synthesized through free radical reaction, the iodine-containing nonmetal catalyst iodine or tetrabutylammonium iodide is used, the raw materials are simple, easily available, cheap, non-toxic and pollution-free to the environment, the dosage of the catalyst is small, thecatalyst has higher specificity for the reaction, synthetic reaction time can be shortened, the problem that the metal catalyst is difficult to separate in the prior art can be well solved, postprocessing difficulty is reduced, yield of the final product is increased, and purity of the final product is improved.

The invention discloses a method for synthesizing 3, 6-dihydro-2H-pyrazine (thiazine) furan-4-boric acid ester. According to the method, tetrahydropyrazole (thiazine) furan-4-ketone serves as the raw material, generates hydrazone with p-toluenesulfonhydrazide, then reacts with NBS/organic alkali to generate alkenyl bromide and next forms Grignard reagent with magnesium metal, after the Grignard reagent is formed, boron reagent is added for a reaction, and the 3, 6-dihydro-2H-pyrazine (thiazine) furan-4-boric acid ester is obtained. By means of the method, ultralow temperature, column chromatography and palladium catalyzed coupling in a literature method are avoided, raw materials are easy to obtain, cost is low, conditions are mild, and the method has potential industrial application and amplification prospect.

The invention discloses a preparation method of sulfonyl-containing completely substituted parazole. The preparation method of the sulfonyl-containing completely substituted parazole comprises the step of carrying out a condensation reaction on 1,3-diketone and aromatic sulfonyl hydrazine as reaction substrates, iodide as a catalyst, peroxy-tertiary butanol as an oxidant, and cobalt acetate tetrahydrate or anhydrous cobalt chloride as an additive in ethyl acetate or benzene as a solvent, so that the sulfonyl-containing completely substituted parazole is obtained. The preparation method disclosed by the invention has the advantages that good and even excellent yield can be realized for multiple aryl sulfonyl hydrazides and 1,3-diketones, and the highest yield can be 97%; compatibility of functional groups of the substrates is high, and application range of the substrates is wide compared with the traditional method; meanwhile, a preparation process is controllable, so that the preparation method disclosed by the invention is applicable to industrial production of the sulfonyl-containing completely substituted parazole.

The invention relates to the technical field of electronic paste, and discloses a method for improving dispersity of photovoltaic panel electronic paste. The method comprises the following steps: preparing nano-copper powder from copper acetate and hydrazine hydrate under proper conditions, treating the nano-copper powder with toluenesulfonyl hydrazine, and aggregating toluenesulfonyl hydrazine on nano-copper tiny agglomerates; countless tiny bubbles are generated by decomposing in hot water, the bubbles burst and gas driving force generated by the bubbles promote tiny agglomerates formed by agglomeration of the nano-copper particles to be dispersed and fully infiltrated, and the sodium p-toluenesulfonate generated after the p-toluenesulfonylhydrazine is decomposed can promote effective infiltration of paste to the nano-copper particles. P-toluenesulfonyl hydrazide can hydrolyze on the surfaces of the nano-copper tiny agglomerates to generate countless small bubbles to crush the tiny agglomerates to be fully dispersed, and the generated sodium p-toluenesulfonate can also promote the slurry to fully infiltrate the nano-copper particles, so that the problem of agglomeration of the filler tiny agglomerates, which is difficult to solve by traditional mechanical stirring and ball milling, is effectively solved; therefore, uniform and stable dispersion of the conductive phase in the electronic paste is realized.

The invention discloses a preparation method for diphenyl ether serial sulfonyl azide compounds. The preparation method comprises taking a diphenyl ether sulfohydrazide compound (I) as a raw material, dropwise adding a sodium nitrite aqueous solution into an alcohol-acid solution system dissolving all of the raw materials, reacting, so as to directly obtain the corresponding diphenyl ether serial sulfonyl azide compound (II) target product. The alcohol in the alcohol-acid solution system is at least one of C1-4 alcohols, and the acid is at least one of hydrochloric acid, sulfuric acid, phosphoric acid, formic acid, acetate and propionic acid. The method avoids currently-used severely-toxic sodium azide and also avoids disadvantages of usage of a large amount of high-boiling-point organic acids, generation of a large amount of waste acid water, and the like. Because the reactions are all homogeneous reactions, the method possesses obvious advantages of being fast in reaction speed, high in yield, easy for recovery and recycling of low-boiling-point alcohol solvents, and the like.

The invention discloses a process method suitable for amplification preparation of 4-(6-aminopyridin-3-yl) substituted piperidine, and belongs to the synthesis field of a medicine intermediate. N-substituted piperidone, aryl sulfohydrazide and 2-amino-5-bromopyridine are subjected to a coupling reaction under a palladium catalyst, and then are subjected to a hydrogenation to obtain 4-(6-aminopyridin-3-yl) substituted piperidine. According to the process, the raw materials in pyridine do not need to be protected; the condensation and the coupling are carried out in the same reaction kettle, sothat the operation cost is reduced, the steps of performing protection at first and then performing protection removal as in documents can be avoided, and production cost of the existing biological, medicine and chemical intermediates is greatly reduced; and the process is subjected to amplification verification in kilogram-scale, and the verification proves that the yield and the product purity are basically equal to those of gram-scale, so that the method can be used as a process for industrial scale production.

The invention relates to a 6-azabicyclo (3.2.1) nonane-3-substituted derivative and a preparation method thereof, which mainly solve the technical problems that the extension of the prior endocyclic compound with 6-azabicyclo (3.23.1) nonane structure in a space structure is limited and the water solubility of the compound is poor. The reaction formula of the 6-azabicyclo (3.2.1) nonane-3-substituted derivative is shown as above. 3-nitrile-6-azabicyclo (3.2.1) nonane compound IV is obtained by adopting 6-azabicyclo (3.2.1) nonane-3-ketone III as raw materials through nitrile addition, and then the compound IV is reacted with ethanol under acid condition to generate ester compound I; or the compound III is reacted with oxyammonia, aminos, hydrazines, amides, sulfonamides, hydrazides or sulfonyl hydrazides to generate compound V, and the compound V is reduced to generate compound II.

The invention discloses a method for synthesizing alkyne sulfone compounds from terminal alkyne and sulfonyl hydrazine. According to the method, a series of the alkynyl sulfone compounds are synthesized through an oxidative cross-coupling reaction of terminal alkyne and sulfonyl hydrazine, and the method does not need pre-functionalization of alkyne, and has the advantages of high atom economy, nometal or oxidant, good functional group tolerance and the like. The compounds synthesized by the method are subjected to in-vitro antitumor activity screening, and experimental results show that mostof the compounds have relatively strong inhibitory activity on tumor cells.

The invention relates to a synthesis method for synthesizing a 3-sulfonylated thioflavonoid compound. The method comprises the following steps: under the action of a catalyst and an oxidizing agent, putting a methylthio aromatic alkyne ketone compound and an aryl sulfonyl hydrazine compound into a solvent, performing reaction under the conditions of blue light irradiation and a nitrogen environment, and performing separation after the reaction is finished, thereby obtaining the 3-sulfonylated thioflavone compound. According to the method, a transition metal catalyst is not needed, a traditional volatile organic solvent is not needed, a green solvent ethylene glycol or water is used as a reaction medium, an organic photosensitizer is used as a catalyst under the catalysis of visible light,and a target product is synthesized through a one-pot reaction. The method is simple, convenient and safe to operate and mild in reaction condition, the light source used in the method is visible light which is green and pollution-free, the catalyst and the reaction medium are environmentally friendly, and in addition, the yield of the product synthesized by the method is high.

The invention relates to a method for preparing a beta-ketosulfone compound through a visible light mediated atopic acid decarboxylation ketonization reaction, and belongs to the field of compound preparation. According to the method disclosed by the invention, environment-friendly atortic acid with wide sources and stable odorless sulfonyl hydrazine are used as reactants, fluorescein, inorganic base and potassium iodide are added and then fully dissolved in a mixed solvent of acetonitrile and water, a reaction is carried out in an oxygen atmosphere (communicated with oxygen spheres), and thebeta-ketosulfone compound can be obtained through the reaction under visible light irradiation. The preparation method disclosed by the invention has the characteristics of simple and easily availableraw materials, simple operation, mild reaction conditions, no metal residue and insensitivity of a reaction system to water.

The invention belongs to the field of new materials, and particularly relates to a super-hydrophobic-lubricating composite anti-icing coating with a porous structure and a preparation method thereof.The coating is composed of a foamed porous super-hydrophobic coating and a bionic joint lubricating liquid, and the super-hydrophobic-lubricating composite anti-icing coating of the super-hydrophobicfoamed porous structure is prepared by compounding low-molecular polybutadiene, polyacrylamide, waterborne polyurethane and alkyl ketene dimer and then heating and foaming p-toluenesulfonyl hydrazine.Blended components of the bionic joint lubricating fluid of the obtained coating and low-molecular-weight polybutadiene can significantly reduce the adhesive force of an ice layer, so that the adhesive force of the ice layer is reduced to 5 kPa or below, and an excellent ice-resistant effect is achieved.

The invention discloses a POE-coated nano argil modified low-density polyethylene (LDPE) foamed material which is prepared from the following raw materials in parts by weight: 60-100 parts of LDPE, 0-40 parts of LLDPE (linear low-density polyethylene), 30-40 parts of POE, 10-20 parts of nano argil, 2-3 parts of vinyltriethoxysilane, 5-10 parts of ammonium polyphosphate, 4-6 parts of p-toluenesulfonhydrazide, 2-3 parts of sodium bicarbonate, 5-8 parts of tributyl citrate, 1-1.5 parts of 2,5-dimethyl-2,5--di(tert-butylperoxy)ethane, 2-4 parts of zinc oxide, 1-2 parts of stearic acid, 1-2 parts of dibasic lead phosphite, 2-3 parts of ethylene-bis-oleamide, 3-5 parts of modified plant ash, 1-2 parts of ultraviolet absorbent UV-0 and 2-3 parts of antioxidant DSTP. The POE-coated nano argil modified LDPE foamed material disclosed by the invention has the advantages of light weight, softness, high strength, favorable resilience, ideal foaming effect, uniform, fine and compact pores, favorable flame retardancy, resistance to chemical attack, aging resistance and high durability.