364results about "Thiol preparation" patented technology

Provided herein is a pleuromutilin derivative containing a cycloalkyl group and preparation method and application thereof. Specifically, the pleuromutilin is reacted with p-toluenesulfonyl chloride to obtain an intermediate I, and the intermediate I is reacted with 1-amino-2-methylpropane-2-thiol hydrochloride to obtain an intermediate II, and then the intermediate II is reacted with cycloalkylcarbonyl chloride to obtain a target derivative. The synthesis process of these derivatives is simple, with a high yield and simple purification. These derivatives can effectively inhibit activities of Staphylococcus aureus and Streptococcus, and have superior activities to the marketed Tiamulin, and they also have good antibacterial activities against drug-resistant bacteria. In particular, the treatment effect of the derivative 2 of the target derivative is significantly superior to the clinical drugs Tiamulin and Valnemulin. They are suitable as new antibacterial drugs for prevention and treatment of infectious diseases caused by bacteria in humans or animals.

The invention discloses a method for preparing 12-mercaptan through solid organic acid catalysis, belongs to the technical field of 12-mercaptan preparation, and aims to solve the problems of low catalyst activity, harsh reaction conditions, serious pollution, high cost and dependence on import in the prior art. N-dodecanol and hydrogen sulfide are used as raw materials and are mixed according to the molar ratio of 1: 1.2-1: 1.3; the method comprises the following steps: gasifying n-dodecanol, mixing with purified hydrogen sulfide, preheating to 210-240 DEG C, introducing into a fixed bed reactor filled with a solid organic acid catalyst, and reacting at-0.08-3.0 MPa for 3.5-4 hours; and cooling and condensing the reaction product, carrying out gas-liquid separation, rectifying and purifying the liquid product to obtain 12-mercaptan with the purity of more than or equal to 99.5%, and recycling unreacted hydrogen sulfide. The solid organic acid can be a catalyst of p-toluenesulfonic acid and the like or mesoporous silica loaded nickel, cobalt and molybdenum metal oxides. The method has the advantages of high catalytic activity, mild reaction conditions, high product yield (the conversion rate of n-dodecanol is greater than or equal to 94.5%), environmental protection and low cost, can realize the domestic mass production of 12-mercaptan, and meets the market demand.

The invention relates to a carbon fiber sizing agent matched with (poly) dicyclopentadiene for use and application of the carbon fiber sizing agent, and belongs to the technical field of poly dicyclopentadiene. The two most important components, namely the coupling agent (component 1) and the film-forming agent (component 2), of the sizing agent are synthesized through a one-pot method, separation, solvent recovery and washing purification are not needed, and the sizing agent is efficient and environmentally friendly. Finally, the introduction strategy of the coupling catalyst (component 3) is optimized, and the reaction efficiency of the carbon fiber and the sizing agent layer is improved to the maximum extent. The method is simple to operate, energy-saving, environment-friendly, high in reaction efficiency and good in interface enhancement effect, can realize batch production of the sizing agent, and can realize batch production of special carbon fibers.

The invention discloses a preparation method and application of a CoxSy catalyst, and belongs to the technical field of catalyst preparation. According to the method, the morphology of CoxSy is regulated and controlled by using different solvents, so that four CoxSy catalysts with different morphology characteristics are synthesized. The catalyst is simple in preparation method and high in repeatability. The obtained CoxSy catalyst has a high specific surface area, more active sites can be exposed, reaction raw materials are in full contact with the active sites of the catalyst, and meanwhile, the catalyst has relatively high sulfur tolerance and rich sulfur vacancies, and is beneficial to adsorption and activation of H2S and CO2. Therefore, the obtained CoxSy catalyst shows high catalytic activity in a reaction for preparing methyl mercaptan through H2S and CO2 hydrogenation.

The invention provides a preparation method and application of a catalyst for selective production of ethanethiol. The catalyst comprises an active component, an auxiliary agent and a molded alumina carrier, the active component comprises the following components in percentage by mass: 5-10% of VIII group transition metal oxide and 15-20% of VIB group metal oxide, and the auxiliaries comprise 0.5-4% of alkali metal, 1-3% of alkaline earth metal oxide, 0.6-2% of cerium oxide and 1-4% of phosphorus pentoxide. A bifunctional catalyst with moderate Lewis acid-base sites is constructed by compounding a multi-component aid and an active component, and the catalyst shows excellent catalytic activity that the ethylene conversion per pass is greater than or equal to 98%, the ethanethiol selectivity is about-95% and the ethanethiol yield is-90% under the reaction conditions that the hydrogen sulfide / ethylene feeding mass ratio is 3-5, the temperature is 180-210 DEG C, the pressure is 0.5-1.0 MPa and the volume space velocity is 200-300 h <-1 >. And the catalyst can stably run for 1250 hours or more.

The invention provides a method for determining the content of penicillamine enantiomers by pre-column derivatization liquid chromatography, namely a method for detecting L-penicillamine in D-penicillamine or a method for detecting D-penicillamine in L-penicillamine, derivatization is carried out under conventional alkaline conditions, a termination reaction is carried out by conventional acid, the derivatization steps are simplified, the detection efficiency is improved, and the detection cost is reduced. According to the method, various interferences of other amino acids and corresponding isomers in the raw materials can be effectively avoided due to the gradient of the mobile phase, the damage to a chromatographic column is well reduced due to the fact that conventional reagents such as phosphoric acid and acetonitrile serve as the mobile phase, and the method is easy to operate, high in sample preparation speed and high in accuracy. The method has the advantages of strong anti-interference capability, good separation effect, high sensitivity, accurate result and good stability, realizes effective separation of penicillamine isomers, has a separation degree of greater than 2, can perform content determination on another main drug while performing impurity detection on one isomer, and has good practicability.

The invention provides a high-temperature-resistant bactericidal corrosion inhibitor as well as a preparation method and application thereof. The preparation method comprises the following steps: reacting a sulfydryl carboxylic acid compound and polyethyleneimine in an organic solvent at a first temperature for a first time to obtain a system containing a first compound; and adding halogenated hydrocarbon into the system containing the first compound, reacting at a second temperature for a second time to obtain a system containing a second compound, removing the organic solvent, and drying to obtain the high-temperature-resistant bactericidal corrosion inhibitor. The high-temperature-resistant bactericidal corrosion inhibitor disclosed by the invention is prepared by the preparation method. The invention also provides an application of the high-temperature-resistant bactericidal corrosion inhibitor in microbial corrosion protection and / or chemical corrosion protection of oil and gas fields. The high-temperature-resistant bactericidal corrosion inhibitor disclosed by the invention is simple in preparation method, good in high-temperature stability and excellent in bactericidal corrosion inhibition performance.

The present invention relates to a method for large-scale production of a benzo [d] thiazole intermediate for preparing torametinib, and a method for large-scale preparation of torametinib using the intermediate, the method avoiding a column chromatography operation which is expensive and complicated to operate while significantly improving the yield of the benzo [d] thiazole intermediate, and the method for large-scale production of torametinib using the intermediate. And thus, the yield of the final product torametinib is improved. Therefore, according to the method, the cost is greatly reduced, the yield is improved, and the method is suitable for large-scale production.

A method of producing pentaerythritol mercaptocarboxylate including subjecting a mercaptocarboxylic acid and pentaerythritol to a dehydration reaction under solvent-free conditions, a polymerizable composition containing the pentaerythritol mercaptocarboxylate, a resin which is a cured product of the polymerizable composition, an optical material containing the resin, and a spectacle lens containing the resin.

The invention relates to a method for catalytically synthesizing 3-mercaptopropionic acid by an MgO-loaded molecular sieve, and belongs to the technical field of organic synthesis. In order to solve the problems that an existing solid-phase catalyst is not easy to regenerate and the selectivity of 3-mercaptopropionic acid is low, the preparation method comprises the following steps: firstly, mixing a roasted molecular sieve, magnesium acetate tetrahydrate powder and distilled water to obtain an impregnated solid mixture, and carrying out temperature programming roasting on the solid mixture to obtain an MgO-loaded molecular sieve catalyst with the MgO loading capacity of 0.5-20%; and mixing the MgO-loaded molecular sieve catalyst, acrylic acid and an organic solvent, introducing hydrogen sulfide, and carrying out a heating reaction to obtain 3-mercaptopropionic acid. The MgO-loaded molecular sieve is used for catalyzing the addition reaction of hydrogen sulfide and acrylic acid to synthesize 3-mercaptopropionic acid, and the selectivity and selectivity of 3-mercaptopropionic acid are both higher than 90%. The MgO-loaded molecular sieve catalyst prepared by the invention has the characteristics of high catalytic activity, simple synthesis and mild catalytic synthesis conditions.

The invention relates to a method for synthesizing 3-mercaptopropionic acid by catalyzing acrylic acid and hydrogen sulfide through an acidic molecular sieve, and belongs to the technical field of organic synthesis. In order to solve the problems of low selectivity and difficulty in regeneration of 3-mercaptopropionic acid prepared from an existing basic catalyst, the method comprises the following steps: firstly, pretreating a molecular sieve catalyst to obtain a required acidic molecular sieve catalyst; and mixing the acidic molecular sieve catalyst, acrylic acid and an organic solvent according to a certain mass volume ratio, introducing hydrogen sulfide to a certain pressure, heating to a reaction temperature, and reacting for a certain time to obtain 3-mercaptopropionic acid. The acidic molecular sieve used in the invention has the characteristics of high catalytic activity, high selectivity, high mechanical strength and reproducibility, and can catalyze the addition of acrylic acid and hydrogen sulfide to synthesize 3-mercaptopropionic acid in one step, the conversion rate of 3-mercaptopropionic acid is higher than 90%, the selectivity is higher than 85%, and the method has the characteristics of simple catalytic synthesis method, mild conditions and the like.

The invention is applied to the technical field of compound preparation, and discloses a synthesis method of o-aminothiophenol, which comprises the following steps: uniformly mixing 2-chloronitrobenzene, water and strongly basic anion exchange resin, heating, dropwise adding a hydrosulfide aqueous solution, carrying out heat preservation reaction, cooling and filtering after the reaction is finished, and drying to obtain the o-aminothiophenol. Eluting the filter cake with liquid alkali, acidifying and layering to obtain an o-aminothiophenol crude product, and distilling to obtain the product. The thiophenol and the basic group of the resin are salified, the main reaction for generating 2-nitrothiophenol is promoted in the early stage, and the generation of a nitroreduction byproduct 2-aminochlorobenzene is greatly reduced, so that the product yield is greatly improved; the product stability is improved by salifying, so that disulfides are prevented from being formed by bimolecular oxidation of thiophenol, reduction is not needed, the product can be obtained by acidification after alkali elution, the process is shortened, and the cost is reduced; the production process is simple to operate, pressure reaction is avoided, the requirement on equipment is low, and the yield is high and can reach 95% or above; the purity of the obtained product can reach 99% or above.

A method for producing a polythiol composition, the method including a reaction step of reacting a thiocarbamate resin with a quaternary ammonium salt comprising a quaternary ammonium cation and a counter anion to produce a polythiol composition.

The invention discloses a bimetallic asymmetric reduction Schiff base catalyst for synthesizing ethylene carbonate and a preparation method of the bimetallic asymmetric reduction Schiff base catalyst. According to the catalyst, a diamine compound is subjected to selective single-side protection, the imine reduction position is controlled, and a bimetallic active center is introduced; the controllable synthesis of a product for reducing the outer side imine and a product for reducing the inner side imine is realized; the obtained product is recrystallized to obtain a monoimine-monoamine type ligand with a clear asymmetric structure, the monoimine-monoamine type ligand and metal salt form a bimetallic catalyst, and the catalyst generates a synergistic effect through double active sites and shows high catalytic activity and excellent product selectivity.

The present invention relates to a method for producing methyl mercaptan, comprising the following steps: A) methanol is reacted with hydrogen sulfide to form a stream (M), preferably in the gas state, comprising methyl mercaptan, unreacted H2S and possibly sulfur-bearing by-products; B) optionally, said stream (M) is condensed; C) at least one step of purifying said stream (M) is carried out in order to obtain a methyl mercaptan-enriched stream; D) the gaseous effluents resulting from said at least one purification step are recovered, said gaseous effluents comprising at least one sulfur-bearing compound, preferably H2S; E) a gas-liquid extraction of said at least one sulfur-bearing compound, preferably H2S, is carried out using liquid methanol so as to obtain a liquid methanol enriched in sulfur-bearing compound(s), preferably in H2S; and F) optionally, said enriched methanol is used as a reactant for the reaction of step A).

The invention relates to a preparation device and method for isooctyl thioglycolate, and particularly to the technical field of chemical intermediate preparation. A synthesis tank and a stirring mechanism are provided, the stirring mechanism is placed in a synthesis space of the synthesis tank, raw materials for isooctyl thioglycolate to be synthesized are placed into the synthesis space of the synthesis tank according to a set molar ratio, a first driving member arranged outside the synthesis tank is connected to a portion of a first stirring member extending out of the synthesis space, and a free end of the first stirring member is connected to a second stirring member via a cross universal joint, a sliding member is slidably sleeved on the outer periphery of the first stirring member, and the sliding member is slidable along the first stirring member until it engages with the cross universal joint. The first driving member drives the first stirring member to rotate, thereby stirring different areas in the synthesis space and uniformly dispersing thioglycolic acid and isooctyl alcohol, thereby improving the manufacturing efficiency of isooctyl thioglycolate.

The invention provides a preparation method of a magnetic recoverable catalyst and a method for synthesizing 3-mercaptopropionic acid, and mainly solves the problem that a large amount of acid and alkali solutions are needed in the existing acrylonitrile-sodium hydrosulfide and acrylic acid-thiourea process routes. The thiohydracrylic acid synthesis catalyst is prepared. The use conditions of the catalyst are as follows: the temperature is 30-80 DEG C, the reaction pressure is 0.5-3 MPa, the mass ratio of the acrylic acid to the solvent is 0.1-5, and the mass ratio of the acrylic acid to the catalyst is 0.2-20. Compared with the prior art, the catalyst disclosed by the invention is used as a synthetic catalyst for preparing thiohydracrylic acid through reaction of acrylic acid and hydrogen sulfide, a solid catalyst and a liquid reaction system can be completely separated by adopting simple methods such as filtration, centrifugation or magnetic separation, and a complicated pickling step is not needed; and the problem that a homogeneous catalyst is difficult to rectify after salification in the use process is avoided.

The present invention provides a polythiol obtained by thiolating a hydroxyl group of a plant-derived polyol.

To provide a novel method for producing a gluconamide derivative, a deoxy-sulfonyloxy gluconamide derivative, a deoxyhalogeno gluconic acid derivative, and a deoxymercapto gluconamide derivative.SOLUTION: In one aspect, a method for producing a gluconamide derivative includes contacting an amine compound with a gluconolactone protector to obtain a gluconamide derivative represented by the formula (3). In another aspect, a method for producing a deoxy-sulfonyloxy gluconamide derivative includes contacting a gluconamide derivative represented by the formula (3) with a sulfonylation agent to obtain a deoxy-sulfonyloxy gluconamide derivative.SELECTED DRAWING: None

The present invention relates to a process for the production of methyl mercaptan comprising the following steps: A) methanol is reacted with hydrogen sulfide to form a stream (M), preferably in the gaseous state, comprising methyl mercaptan, unreacted H2S and optionally sulfur by-products; B) optionally, said stream (M) is condensed; C) at least one purification step of said stream (M) is carried out to obtain a stream enriched in methyl mercaptan; D) the gas vents from said at least one purification step are recovered, said gas vents comprising at least one sulfur compound, preferably H2S; E) a gas-liquid extraction of said at least one sulfur compound, preferably H2S, is carried out with liquid methanol to obtain a liquid methanol enriched in sulfur compound(s), preferably H2S; and F) possibly, said enriched methanol is used as a reagent for the reaction in step A).

The invention relates to a full bio-based Schiff base type epoxy curing agent as well as a preparation method and application thereof, the chemical structural formula of the epoxy curing agent is # imgabs0 #, in the formula, R1 is-H or-O-CH3; compared with the prior art, the epoxy resin has the advantages that the raw materials can be completely obtained by converting biomass resources, the preparation method is simple, and the cured epoxy resin is excellent in performance.

The present application belongs to the technical field of condensate, and particularly relates to a non-peptide small molecule condensate and preparation and application thereof. The present application provides a non-peptide small molecule condensate which is prepared by taking a small molecule shown in formula I as a precursor, wherein Y and Z are each independently NH, O or S, R = or X = O or S; R1 and R2 are each independently selected from H, C 3‑20 alkyl, -C 1‑8 alkylene-phenyl, -C 1‑8 alkylene-5-10-membered heteroaryl, -C 1‑8 alkylene-S-C 1‑8 alkyl, -C 1‑8 alkylene-SH, -C 1‑8 alkylene-O-C 1‑8 alkyl or -C 1‑8 alkylene-NH-C 1‑8 alkyl; and R1 and R2 are not H at the same time. The obtained condensate not only has good spontaneous non-classical fluorescence characteristics, but also has the abilities of drug loading and controllable release, and shows excellent resistance to enzymatic hydrolysis and good biocompatibility. Formula I

The present invention discloses a copper-cysteine complex, a preparation method thereof and an application thereof. In the present invention, a soluble copper salt, L-cysteine and deionized water are mixed by a one-pot method, stirred, the pH is adjusted, and the temperature is raised to reflux by boiling to obtain the copper-cysteine complex. The copper-cysteine complex prepared by the present invention has excellent luminescence properties, good water dispersibility and excellent free radical generation ability.

The polythiol composition according to an exemplary embodiment includes a tetrafunctional polythiol compound and a parapolythiol compound, the parapolythiol compound comprising C 13 H 28 S9 represents compounds and compounds derived from C 15 H 32 S 10 The compounds are indicated. The proportion of parapolythiol compounds, as measured by high-performance liquid chromatography (HPLC), ranges from 1% to 5%. By adjusting the content of parapolythiol compounds, optical products with excellent transmittance and optical properties can be manufactured.

A method for producing a high purity product sulfide from an olefin is provided. 【Solution means】Hydrogen sulfide or R 1 SH, and a method for producing a high purity product sulfide from an olefin of the formula C x H (2x) comprising the steps of: feeding hydrogen sulfide or R 1 SH, and an olefin of the formula C x H (2x) to a reactor system; separating the reactor effluent stream into a first portion and a second portion; recycling the first portion of the reactor effluent stream to the reactor system; and feeding the second portion of the reactor effluent stream to a sulfide separation system, the sulfide separation system comprising: at least one recycle stream comprising at least a portion of unreacted hydrogen sulfide, unreacted olefin of the formula C x H (2x) unreacted R 1 SH, and other components, and a product stream comprising the high purity product sulfide.

This invention provides a tert-nonylthiol and its synthesis method. The synthesis steps are as follows: nonene and hydrogen sulfide are preheated separately, then the preheated nonene and hydrogen sulfide are mixed, and the mixture is reacted under the action of a catalyst to obtain tert-nonylthiol. The preheating temperature of nonene is 40-50℃, and the preheating temperature of hydrogen sulfide is 50-60℃. This invention provides mild reaction conditions and precise preheating of nonene and hydrogen chloride separately. The product prepared by this method has a purity of over 99.0%, meeting the requirements of high-end industrial applications for high-purity tert-nonylthiol.

The present invention disclosed 3-substituted phenylamidine compounds of general formula (I), wherein R1, R2, R3, R4, R4a, R4b, A and E have the same meanings as defined in description. The present invention further discloses methods for their preparation and use of the compounds of general formula (I) as a crop protection agent.

The invention relates to the technical field of chemical material preparation, and particularly discloses a safe preparation method of a short fluorocarbon alkyl sulphobetaine surfactant, a product and application, and the safe preparation method comprises the following steps: (1) in a solvent system I, reacting epoxy chloropropane with secondary amine to obtain an intermediate 1; (2) in a solvent system II, reacting the intermediate 1 with sodium hydrosulfide or a hydrate thereof to obtain an intermediate 2; (3) reacting the intermediate 2 with short fluorocarbon alkyl iodide to obtain perfluoroalkyl thioether propyl tertiary amine; and (4) carrying out sulfonation treatment on perfluoroalkyl thioether propyl tertiary amine to obtain the short-fluorocarbon alkyl sulphobetaine surfactant. According to the invention, by designing a synthetic route without using a high-risk reagent, the safety and operability of the process are remarkably improved, and the sulphobetaine surfactant with excellent acid, alkali and salt chemical stability and excellent surface activity is successfully prepared; and a key material and a safe and reliable preparation process are provided for development of a new-generation efficient environment-friendly fire extinguishing agent.

The present invention relates to the field of organic synthesis, and discloses an ester compound synthesis method, which comprises: mixing an organic acid raw material and an organic alcohol raw material, and carrying out a reaction under the action of a homogeneous catalyst to obtain an ester compound, the mixing index of the organic acid raw material and the organic alcohol raw material being greater than or equal to 0.9 after the organic acid raw material and the organic alcohol raw material are mixed. According to the method, the conversion efficiency of the ester production process is improved by accurately controlling the mixing index of the esterification reaction system.