110results about How to "Simple and mild reaction conditions" patented technology

The invention relates to in-situ crosslinked alginate hydrogels with an active ingredient of disulfide bond disulfide bond alginate derivative. The preparation method thereof is as follows: the organic liquids of carbodiimide hydrochloride and N-hydroxysuccinimide eater are added into the alginate aqueous liquid of the alginate to activate the carboxyl of the alginate aqueous liquid; then the organic liquid of 4-aminothiolphenol is added under the conditions of keeping in dark place under 10 DEG C and nitrogen protection, so that the amino of the 4-aminothiolphenol and the carboxyl of the alginate aqueous liquid form an amido bond. The proportions of each matter adjusted and the pH value of muriatic acid is adjusted to 6.0, ethanol is deposited, frozen and dried to obtain sulfhydrylation alginates of different sulfydryl contents. The alginate aqueous liquid of the alginate oxidizes the sulfydryl thorugh the oxygen in the liquid under a room temperature to crosslink and form a disulfide bond, thus obtaining the crosslinked alginate hydrogels. The hydrogels prepared through the method has pH sensitivity and reduction responsiveness, and has potential application values in drug delivery field.

The invention discloses a synthesis method of beta, beta-diaryl alkene, which comprises the following steps that: in an organic acid solvent, in the presence of a palladium catalyst and a silver salt, a halogenated aromatic hydrocarbon and an end alkenyl compound are subjected to a coupling reaction to obtain the beta, beta-diaryl alkene, wherein the organic acid solvent is acetic acid, the palladium catalyst is palladium acetate, the silver salt is silver acetate, silver carbonate or silver oxide, the halogenated aromatic hydrocarbon is iodo aromatic hydrocarbon, and the coupling reaction is operated at a reaction temperature of 80 to 130 DEG C for 0.25 to 24 hours. With the method, the environmentally friendly organic acid is used as the solvent, and the silver salt is used as an additive; and the method has the advantages of small amount of catalyst, mild reaction conditions, simple post-treatment, and high yield of a product, without adding other ligands and the like.

The invention discloses a method for catalytically asymmetrically synthesizing a chiral beta-aminoketone derivative. The method includes taking a chiral binaphthol derivative shown in a formula (3) asa catalyst; and in the presence of an organic solvent and an additive, preforming, by potassium trifluoroborate shown in a formula (2), an asymmetric 1,4-addition reaction on a beta-phthalimide acrylone compound shown in a formula (1) to generate the beta-aminoketone derivative containing one chiral center shown in a formula (4), wherein the reaction formula is shown in the specification. The invention discloses a new chiral catalyst of a polyfluoroaphthol skeleton, adopts nonmetallic catalysis, avoids the use of metal catalysts from the source, and reduces the reaction cost. The yield and enantioselectivity of the target product are high, the reaction conditions are simple and mild, and a method for preparing multiple chiral beta-aminoketone derivatives is provided, so that the method has better application prospect and social value.

The invention discloses a magnetic mesoporous carbon-supported cobalt catalyst and a preparation method and application of the catalyst. The magnetic mesoporous carbon-supported cobalt catalyst takes magnetic mesoporous carbon as a carrier, a cobalt ion is fixed into the magnetic mesoporous carbon through an isopyknic immersion method, and the weight percent of cobalt is 2.5%-4.5%. The preparation method particularly comprises the steps of preparing the magnetic mesoporous carbon by adopting a template method; dripping ultrapure water to the magnetic mesoporous carbon to obtain saturated water-absorbing capacity of the magnetic mesoporous carbon; then dripping a cobalt nitrate solution with saturated water-absorbing volume to the magnetic mesoporous carbon, immersing for 24-36 hours to obtain the magnetic mesoporous carbon immersed with cobalt; drying the magnetic mesoporous carbon immersed with the cobalt, grinding the dried magnetic mesoporous carbon into powder, and calcining to complete the preparation of the magnetic mesoporous carbon-supported cobalt catalyst. The magnetic mesoporous carbon-supported cobalt catalyst provided by the invention adopts a simple preparation method, can be separated by using a magnet after being used and can be repeatedly used, has high degradation efficiency on an azo dye and has no secondary pollution and can be used for degrading the azo dye.

The invention discloses a method for synthesizing a 3-hydroxyl oxoindole derivative. The synthetic route is as shown in the specification, wherein R1 is methyl, ethyl, propyl, butyl, isopropyl, cyclohexyl, allyl, benzyloxyethyl or n-butyric acid methyl ester; a substituent R2 is methyl, methoxy, benzyloxy, fluorine, chlorine or bromine; and a substituent R3 is methyl, bromine or phenyl. The synthetic process comprises the following steps: dissolving a compound I and iodobenzene diacetate in acetic acid and reacting completely at 40-100 DEG C, and postprocessing and purifying to obtain a product II. The raw materials used in the method are easy to prepare, and iodobenzene diacetate can be sold in the market; there is no need to use a catalyst such as a metal catalyst or an organic catalyst, and cost is reduced and the method is environment-friendly.

The invention discloses a preparation method of a block copolymer with dual responsiveness of rapid oxidization / reduction and selenium bonds and application of the block copolymer. The preparation method comprises the following steps: firstly preparing diazido-terminated double-selenium micromolecules (N3-SeSe-N3) and dipropargyl-terminated polyethylene glycol (PA-PEG-PA); obtaining alternating copolymer (PA-PEGalt-SeSe-PA) containing double selenium bonds and polyethylene glycol, wherein two ends of the alternating copolymer are terminated by alkynyl; then reacting the alternating copolymer (PA-PEGalt-SeSe-PA) with azido single-terminated polycaprolactone (PCL-N3) to obtain the block copolymer (PCL-PEGSeSe-PCL) with dual responsiveness of rapid oxidization / reduction and double selenium bonds; a nanoparticle self-assembled by the amphiphilic copolymer in an aqueous solution has high biocompatibility and biodegradability; the nanoparticle is coated with a hydrophobic anti-cancer drug; the polymer nanoparticle can be broken in the tumor cell environment for rapidly releasing the coated drug, so that the block copolymer has potential application prospects in the aspect of cancer therapy.

The invention discloses a hydrangea-shaped gold nanoparticle and a preparation method of the hydrangea-shaped gold nanoparticle. The method includes the steps that a chloroauric acid solution is added into a surface active agent hexadecyl trimethyl ammonium chloride solution, and magnetic stirring is performed; then an ascorbic acid solution is added, magnetic stirring is performed, growth temperature is adjusted and controlled, standing growth is performed, and the hydrangea-shaped gold nanoparticle is obtained through purification after an obtained solution is centrifuged and washed. The average diameter is 490 nm-812 nm, and the thickness of pedals is 20 nm-44 nm. The prepared gold nanoparticle is of the hydrangea-shaped structure and is high in yield and good in monodispersity and stability, the appearance and the optical property of the particle are controllable and adjustable, and the gold nanoparticle further has the advantages of being simple in synthetic method, mild in synthetic condition, good in stability and the like.

The invention provides a method for treating residual atrazine in a water body by LaFe(1-x)CuxO3. The method comprises steps as follows: peroxymonosulfate is added to organic wastewater and mixed uniformly, then a LaFe(1-x)CuxO3 material is added and serves as a heterogeneous catalyst, all components are stirred, and atrazine pollutants are degraded accordingly; concentration of peroxymonosulfatein the organic wastewater is 0.25-1 mmol / L. According to the method, LaFe(1-x)CuxO3 is taken as the heterogeneous catalyst and is subjected to a reaction with to-be-treated atrazine in the coexistenceof both LaFe(1-x)CuxO3 and peroxymonosulfate, Fe(III) / Fe(II) and Cu(II) / Cu(I) in the LaFe(1-x)CuxO3 material are taken as main active components and subjected to a contact reaction with peroxymonosulfate, sulfate radicals with strong oxidizing property are produced, atrazine which is difficult to degrade in the water body is degraded by the sulfate radicals, and therefore, the water body is purified.

The invention discloses a preparation method of quercetin-loaded nano-selenium. The quercetin-loaded nano-selenium comprises the following raw materials: a reducing agent, a reaction solution and a selenium source, wherein quercetin is used as the reducing agent, sodium selenite (Na2SeO3) is used as the selenium source, the reaction solution contains a stabilizer and a mixed solvent of methanol and water, and the stabilizer is gum arabic (As). The preparation method comprises the following specific steps: preparing nano selenium particles for loading quercetin, firstly preparing the reaction solution containing the stabilizer, adding quercetin and sodium selenite substance into the reaction solution, stirring and reacting for a period of time at room temperature, then adding a proper amount of tween 80, continuously stirring, removing methanol by rotary evaporation, and freeze-drying to obtain the quercetin-loaded nano-selenium. The invention further discloses application of the quercetin-loaded nano-selenium in treating Alzheimer's disease. The invention aims to provide a preparation method and application of a medicament for treating Alzheimer's disease.

The invention discloses a method of using alkaline earth metal hydrides to reduce carbon dioxide to prepare a hydrogen-methane mixed fuel. According to the method, in an argon atmosphere, alkaline earth metal hydrides are placed in a ball mill tank, argon is extracted from the ball mill tank, highly pure CO2 gas is filled into the ball mill tank, and a ball milling machine is adopted to carry out ball milling reactions at a room temperature to obtain the hydrogen-methane mixed fuel. The method can prepare hydrogen-methane mixed gas at a room temperature, a novel method is provided for high density storage and preparation of methane, and a novel technology, which can carry out carbon dioxide methanation under mild conditions, is also provided.

The invention discloses a method for preparing 7-amino-3-sulfotetrazolthiomethylcephalosporanic acid, which comprises: adding solution of boron trifluoride and dimethyl carbonate in a dimethyl carbonate solvent, stirring the solution, adding 7-aminocephalosporanic acid and 5-mercapto-1H-tetrazole-1-methanesulfonic acid disodium salt in turn to perform an reaction; when reactant residue is less than or equal to 0.5 percent, adding purified water to continue the reaction; cooling the reaction solution, filtering the reaction solution, and washing the product obtained by filtration to obtain a coarse crystal product; and dissolving the coarse crystal product, adding an organic solvent, adjusting the pH value, stirring the solution, cooling and standing the solution, filtering the solution, washing the product obtained after filtration and drying the product to obtain the finished product. Compared with the traditional process, the method has the advantages of mild and simple reaction conditions, easy solvent recovery and recycling, reaction yield up to 90 to 91.2 percent, purity up to 98.0 percent and light color as the solution of boron trifluoride and dimethyl carbonate is used as a catalyst. The method is suitable for large-scale production and overcomes the drawbacks of high price, difficult recovery, low yield, low purity and high production cost of the process using solution of boron trifluoride and acetonitrile as a catalyst.

The invention discloses a method for preparing an oxazoline insecticide arfamarin intermediate. The intermediate is 4-formyl-naphthalene-1-carboxylic acid, and compared with a synthesis route of US6613942B1, the synthesis route of the oxazoline insecticide arfamarin is simple. According to the method provided by some embodiments of the invention, through exploration, the reaction steps are shortened from three steps to one step, so the oxazoline insecticide arforlaana intermediate product with qualified purity can be obtained. The intermediate control steps are simplified, meanwhile, the product yield is increased, and industrial production is easier.

The invention discloses a preparation method of tetraethyl methylene diphosphate, comprising the following steps: 1) under the action of sodium ethoxide, diethyl phosphite reacts with sodium ethoxide to obtain sodium diethyl phosphite ethanol solution , ethanol is removed by distillation under reduced pressure to obtain sodium diethyl phosphite solid; 2) dichloromethane is added to the solid sodium diethyl phosphite obtained in step 1); sodium diethyl phosphite and dichloromethane are substituted After the reaction, tetraethyl methylene diphosphate was obtained. The preparation method of the invention has mild and simple reaction conditions and high yield at the same time. The method is simple to operate and low in energy consumption, and is suitable for industrial production.

The invention discloses N, N'-alkylene bis(saturated fatty amide) and a synthesis method thereof. Saturated fatty acid short chain alcohol ester and alkylene amine as raw materials undergo a reaction in the presence of solid Lewis acid as a catalyst to produce the N, N'-alkylene bis(saturated fatty amide). Through use of the saturated fatty acid short chain alcohol ester as a raw material for synthesis of the alkylene bis(saturated fatty amide), raw material reaction activity is improved, a raw material cost is reduced and a cost is saved. Through use of the solid Lewis acid as a catalyst, an amine value and an acid value of the N, N'-alkylene bis(saturated fatty amide) can be adjusted and are obviously lower than those of a N, N'-alkylene bis(saturated fatty amide) synthesized by other catalysts so that the technical problem that color value index of the N, N'-alkylene bis(saturated fatty amide) can be controlled difficultly and the color is yellow is solved, product quality can be improved and product color and luster are improved.

The invention belongs to the field of nucleic acid marking, and particularly relates to a light-click-reaction-based DNA marker with fluorescent responses, a preparing method thereof and an application thereof. The DNA marker is at least one of a compound W-3 and a compound W-4. The structural formula of the W-3 and the structural formula of the W-4 are shown as the formula I and the formula II (please see the specification for the formula I and the formula II). The preparing method is simple and moderate, oxygen and water have no influences on reacting in the reacting process, operation is easy, popularization is easy, and the DNA marker, the preparing method and the application can be applied to the field of nucleic acid marking.

The invention relates to in-situ crosslinked alginate hydrogels with an active ingredient of disulfide bond disulfide bond alginate derivative. The preparation method thereof is as follows: the organic liquids of carbodiimide hydrochloride and N-hydroxysuccinimide eater are added into the alginate aqueous liquid of the alginate to activate the carboxyl of the alginate aqueous liquid; then the organic liquid of 4-aminothiolphenol is added under the conditions of keeping in dark place under 10 DEG C and nitrogen protection, so that the amino of the 4-aminothiolphenol and the carboxyl of the alginate aqueous liquid form an amido bond. The proportions of each matter adjusted and the pH value of muriatic acid is adjusted to 6.0, ethanol is deposited, frozen and dried to obtain sulfhydrylation alginates of different sulfydryl contents. The alginate aqueous liquid of the alginate oxidizes the sulfydryl thorugh the oxygen in the liquid under a room temperature to crosslink and form a disulfide bond, thus obtaining the crosslinked alginate hydrogels. The hydrogels prepared through the method has pH sensitivity and reduction responsiveness, and has potential application values in drug delivery field.

The invention relates to a preparation method of a p-hydroxybenzhydrazide compound. The preparation method comprises the following steps: sequentially adding a catalyst Ag2O, a reactant I, a reactantII and water into a reactor, and putting the reactor into an ice bath for a reaction for 0.5-10 hours; and extracting a reaction solution with an organic solvent, carrying out reduced-pressure distillation on an organic phase to obtain a crude product, and carrying out column chromatography separation and purification to obtain the p-hydroxybenzhydrazide compound. According to the method, raw materials are cheap and easy to obtain, reactions are carried out in a water phase of a green solvent, reaction time is short, reaction conditions are simple and mild, regioselectivity is good, and the produced p-hydroxybenzhydrazide compound has important application value in organic synthesis.

The invention relates to a device and a method for preparing monodisperse calcium alginate microspheres and application. The device comprises an inner-phase glass tube, a middle-phase glass tube and an outer-phase glass tube which are coaxially arranged, the inner-phase glass tube penetrates through a second dispensing needle head to be inserted into the middle-phase glass tube, the middle-phase glass tube penetrates through a third dispensing needle head to be inserted into the outer-phase glass tube, the outer-phase glass tube extends into a collection culture dish, the inner-phase glass tube is communicated with an inner cavity of the first dispensing needle head, the middle-phase glass tube is communicated with an inner space of the second dispensing needle head, the outer-phase glasstube is communicated with an inner space of the third dispensing needle head, and the first dispensing needle head, the second dispensing needle head and the third dispensing needle head are fixedly connected with the bottom plate. The device and the method can be used for preparing the calcium alginate microspheres with better sphericity.

The invention provides a preparation method of sargassum fusiforme dietary fiber. The method includes the steps of: drying, enzymolysis, acidolysis, alkaline hydrolysis, centrifugation, gelation, bleaching, drying, activation, alcohol dehydration and drying. The method provided by the invention employs a composite plant hydrolase to assist papain to extract sargassum fusiforme dietary fiber, greatly improves the protein hydrolysis rate of sargassum fusiforme, overcomes the disadvantage of poor one-time protein removal effect in common enzymatic method, effectively destroys cell walls, enhancesthe full permeation of a fiber crystalline area, completely releases part of the protein closely combined to residue, and is conducive to degradation of papain to protein so as to improve the productpurity.

The invention discloses a fluorine titanium hybrid flame retardant, and a preparation method and application thereof. The fluorine titanium hybrid flame retardant is characterized in that the fluorine titanium hybrid flame retardant has the molecular structural formula shown in the description, wherein R is CH3CH2CH2CH2 or shown as the description. When the fluorine titanium hybrid flame retardant is used for preparing flame-retardant epoxy resin, the reaction conditions are simple and mild; the yield is high; the product purification operation is simple; the industrialization is easy; the prepared epoxy resin has high transparency; on the premise of ensuring the excellent heat resistance and mechanical property, the flame retardant effect is good; the application range is wide; the environment protection requirements are met.

The invention firstly reports a novel synthesis method for obtaining various tetrahydrofuranoindole compounds by performing 1, 1-carbon alkoxylation on gold-catalyzed propynylamine compounds, performing external cyclization at room temperature to obtain external-ring gold carbene, migrating the external-ring gold carbene to gold carbene through 1, 2-H, and constructing and obtaining various tetrahydrofuranoindole compounds by a high-atom economy and diversity strategy. According to the method, the ternary nitrogen-containing heterocyclic compound is obtained only through one-step reaction construction, the reaction only needs to be carried out at room temperature, no additional auxiliary agent is needed, the reaction can be completed in only one hour, the reaction conditions are mild and simple, the efficiency is high, the yield of a target product is high, and the adaptability of a reaction substrate group is good.

The invention discloses a method for preparing lithium cobalt oxide nanosheets. The method includes steps of mixing cobalt salt and strong alkali, heating and centrifuging to obtain dark-blue liquid containing cobalt, and performing heat reaction between the dark-blue liquid containing cobalt and lithium brine so as to obtain the lithium cobalt oxide nanosheets with self-support structures. The method is simple and easy to operate and has a potential industrialization prospect. Products prepared by the method are high in charge and discharge capacity.

The invention relates to a synthesis method for a polybrominated benzene [1.3] oxazine derivative, comprising the following steps of: carrying out reaction of compounds shown in formula (I) and N-bromo-succinimide (NBS) in a solvent at 25-100 DEG C to obtain the polybrominated benzene [1.3] oxazine derivative shown in formula (II) after the reaction is completed. The compounds shown in the formula(I) and the formula (II) are as shown in the description, wherein R is chosen from phenyl, substituted phenyl, C1-C5 alkyl (preferably isopropyl) or thiophene. The synthesis method has the advantagesof being mild in reaction conditions, environment-friendly, simple in operation and capable to obtain polybrominated benzene oxazine compounds which cannot be obtained by conventional methods throughone pot multi-step reaction.

The invention discloses a kinetic resolution method of aryl allyl tertiary alcohol catalyzed by chiral phosphoric acid. In the presence of a solvent and an additive, an allyl tertiary alcohol compound as shown in a formula I is catalyzed by a chiral phosphoric acid catalyst as shown in a formula II, an aryl allyl tertiary alcohol compound, shown as a formula III, and a dihydroisobenzofuran compound, shown as a formula IV, with chiral centers respectively are generated bykinetic resolution, and the reaction equation is also shown. According to the invention,chiral phosphoric acid is used as the catalyst, an aryl allyl tertiary alcohol compound with high functional group compatibility and stable property is used as a catalytic substrate, and under the action of an additive, various chiral aryl allyl tertiary alcohol and dihydroisobenzofuran compounds are prepared. The preparation method disclosed by the invention is high in enantioselectivity and wide in substrate application range, and the obtained chiral aryl allyl tertiary alcohol with high optical activity and the dihydroisobenzofuran containing the tetra-substituted carbon chiral center have extremely high scientific research value and wide application prospect.

The invention relates to a biological enzyme catalysis synthesis method for 6-bromoindanone, and belongs to the field of biological pharmacy. Transpeptidase site-specific mutagenesis type transpeptidase with a SEQ ID NO.2 amino acid sequence has an amino acid sequence disclosed by SEQ ID NO.1, then, propionic acid is added into methyl alcohol to be stirred and fully dissolved, monopotassium phosphate buffer solution of which the pH is 2.0 and 0.95KU site-specific mutagenesis type transpeptidase are added and are stirred for 20h at a room temperature, and after solvent is dried by distillation,filtering is carried out to obtain a crude product; and then, through methyl alcohol / water recrystallization, a 6-bromoindanone competitive product is obtained. An active transpeptidase enzyme prepared by an enzymatic mutation technology is adopted to replace a traditional chemical synthesis process. A reaction condition is moderate and simple, and extremely few three wastes are generated. Compared with a traditional chemical synthesis method, the biological enzyme catalysis synthesis method has higher synthesis efficiency, high yield and high purity.

The invention relates to a preparation method of a p-amino substituted phenol compound. The preparation method comprises the following steps: sequentially adding a catalyst Ag2O, a reactant I, a reactant II and water into a reactor, and putting the reactor into an ice bath to react for 0.5-10 hours; and extracting the reaction solution with an organic solvent, carrying out reduced pressure distillation on the organic phase to obtain a crude product, and carrying out column chromatography separation and purification to obtain the p-amino substituted phenol compound. Reaction conditions and rawmaterials are cheap and easy to obtain and are carried out in a green solvent water phase, the reaction time is short, the reaction conditions are simple and mild, the regioselectivity is good, and the product has important application value in organic synthesis.

The invention provides a preparation method of cinnamaldehyde diethylacetal. The preparation method comprises the following steps: using 2-bromo-1, 1-diethoxy ethane and benzaldehyde as raw material; and, synthesizing cinnamaldehyde diethylacetal through microwave radiation by taking triphenylphosphine as catalyst and solid carrier, wherein the solid carrier is alkaline macroporous resin. According to the preparation method, raw materials are cheap and easy to obtain, solid catalyst can be removed easily, the reaction condition is soft and simple, side reaction is less, the post-treatment is easy, the product yield and purity is high, the cost is greatly reduced, and the continuous production can be carried out.

The invention discloses a trifluoromethanesulfonyl alkyne amide compound as well as a preparation method and application thereof. Based on hydrosulfide reaction of the alkyne amide and sulfydryl, selective modification and marking of sulfydryl in polypeptide and protein are realized. The compound has good stability. Reaction with sulfydryl only can be selected, and other active groups on the polypeptide or protein are not affected; the method has the advantages of high reaction rate, no side reaction, simple and mild reaction conditions, easiness in operation, wide substrate applicability, high atom economy and the like. The compound has good stability under acid-base and oxidation conditions, can stably exist for several months at normal temperature, and provides a new steady way for selective modification and marking of sulfydryl in biological coupling, polypeptide and / or protein.

The invention discloses a method for directly preparing N,N-bislactose-1,10-decamethylene diamine by adopting one-pot reaction, belonging to the technical field of synthesis of glycosyl surfactants. The method comprises the steps of: mixing lactose with decamethylene diamine in a molar ratio of (2.0-2.5):1, adding an alcohol and water mixed solvent with a volume ratio of alcohol to water being (50-75):100, wherein the ratio of the total mass of the lactose and the decamethylene diamine to the mass of the mixed solvent is 1:(4-6); and mechanically stirring for 20-24h at a normal temperature, heating to 45-60 DEG C in a water bath, reacting for 1-2h, cooling and placing for 0.5-2h, separating out a large quantity of solids, filtering, washing, re-crystallizing with absolute ethyl alcohol, freezing and drying to obtain a white solid, i.e. N,N-bislactose-1,10-decamethylene diamine. The method has the advantages of low price and easy obtaining of raw materials, simple and mild reaction conditions, convenience and safety in operation, simpleness in post-treatment, high production yield, suitability for industrial production, and high implementation value.

The invention relates to a preparation method of tetrasodium glutamate diacetate, belonging to the technical field of organic synthesis. The preparation method comprises the following steps: with sodium glutamate, glyoxylic acid and formic acid as raw materials, subjecting glyoxylic acid and sodium glutamate to a sufficient reactionat a certain temperature, and then generating an aqueous tetrasodium glutamate diacetate solution under the action of formic acid. According to the invention, sodium glutamate, glyoxylic acid and formic acid used in the method are easily available raw materials, byproducts are mainly water and carbon dioxide, highly toxic substances such as cyanide and the like are abandoned, and generation of a large amount of wastewater and toxic byproducts are avoided; usageof chloroacetic acid as a raw material is also discarded, so the influence of chloride ions in the product on some use scenes is prevented; and the method is green, economical, environment-friendly and easy for large-scale industrial production.