94 results about "1,4-Dioxane" patented technology

The invention discloses a sulfide functionalized covalent organic frame material, The material has a structural unit shown in the specification, and is obtained by the following steps: adding 2,5-Bis(3-(ethylthio)propoxy)-terephthalohydrazide and benzenetricarboxaldehyde into a mixed solvent of 1,4-dioxane and mesitylene, adding an aqueous acetic acid solution into the above mixture and reacting at 120 DEG C for 1-3 days. The material has a mesoporous structure, has BET specific surface area of 470-480 m<2>?g<-1>, has good selective identification for mercury ions, and can be used for removal of the mercury ions.

The invention discloses a probe reagent for concurrent selection and determination of multiple metal ions, and preparation and appliance, and belongs to the field of organic synthesis and analytical chemistry. Tri (2-aminoethyl) amine serves as a parent, wherein rhodamine B is connected to an amino chain, 2-hydroxy-1-naphthaldehyde groups are connected to other two amino chains respectively, and thus a tripod structured rhodamine-hydroxyl naphthalene derivative probe is prepared. In 1,4-dioxane/water (19/1, v/v, pH=7) solution, the probe respectively detects Cu2+, Co2+ and Fe3+ by utilizing rate absorption of different wavelengths, and the detection does not interfere with each other; in acetonitrile/water (19/1, v/v) solution, fluorescence emission of different wavelengths under different pHs is utilized, the probe respectively detects Zn2+, Al3+, Hg2+ and Cu2+, and the detection does not interfere with each other; under an ultraviolet lamp of 365 nm, Zn2+, Al3+ and Hg2+ are detected to show blue, pink and orange red fluorescence respectively, and through -Zn2+ mixture detection by the probe, Cu2+ shows blue fluorescence vanishing. The probe structure is as follows.

The invention discloses a preparation method of a segmented copolymer from a vinylidene chloride copolymer and polyethylene glycol which comprises the steps of: reacting polyethylene glycol (PEG) and a reversible addition fragmentation transfer radical polymerization (RAFT) chain transfer reagent in dichloromethane under the action of a catalyst 4-dimethylamino pyridine to obtain a PEG macromolecular RAFT reagent; and performing RAFT polymerization on vinylidene chloride or vinylidene chloride and a comonomer in the PEG macromolecular RAFT reagent under the action of azo-bis-iso-butyrynitrile initiator and with 1,4-dioxane as a solvent to obtain a segmented copolymer from a vinylidene chloride copolymer and polyglycol with large molecular weight and narrow molecular weight distribution width. The invention provides a novel method for preparing a vinylidene chloride segmented copolymer, and the segmented copolymer composed of a vinylidene chloride copolymer and polyglycol prepared by the invention has a potential application preparation of hydrophilic modified vinylidene chloride films and vinylidene chloride polymer based mesoporous carbon.

The invention discloses a bioactive bone repair material containing williams elder twig as well as a preparation method and application thereof, and belongs to the field of bone repair materials. The preparation method of the bioactive bone repair material containing williams elder twig comprises the following steps: adding 4g of PLGA and 2g of TCP into 40ml of 1,4-dioxane, and dissolving and stirring for 24 hours; and adding 2mg to 0.4g of williams elder twig active components into 10ml of 1,4-dioxane, dissolving, then adding 1ml of a williams elder twig dissolved solution into an obtained solution, and then stirring for 2 hours to obtain the bioactive bone repair material containing williams elder twig. The bioactive bone repair material containing williams elder twig, disclosed by the invention, can be subjected to three-dimensional printing to form an artificial bone by virtue of a low-temperature fused deposition production and molding technology; and an obtained artificial bone material can be used for releasing an estrogen-like traditional Chinese medicine namely williams elder twig in an absorption process, and can be used for slowing down the bone loss rate of patients suffering osteoporosis; and meanwhile, the bioactive bone repair material containing williams elder twig has biocompatibility and bone inducing ability.

The invention discloses a cheap and efficient synthesis method of an alpha-hydroxyketone compound. The synthesis method is characterized in that a carbonyl compound undergoes an oxidation hydroxylation reaction at 10-120DEG C under normal pressure with iodine simple substance, N-bromosuccimide, copper bromide, bromine simple substance, hydrogen bromide, N-iodosuccimide or hydrogen iodide as a catalyst, sulfoxide as an oxidant, water or sulfoxide as a hydroxy source and sulfoxide, ethyl acetate, N,N-dimethyl formamide, acetonitrile, toluene, 1,4-dioxane, 1,2-dichloroethane, tetrahydrofuran or H2O as a solvent, and converts into the alpha-hydroxyketone compound in a high selectivity manner. Compared with traditional synthesis methods, the method disclosed in the invention has the advantages of simple operation, high yield, simple conditions, easy purification, small waste discharge amount, simple reaction apparatus, and easy industrial production. The method has wide applicability and can be used for synthesizing various alpha-hydroxyketone compounds.

The invention discloses a preparation method of a fluorine-containing high-molecular surfactant, and the preparation method comprises the following steps: enabling an initiator, methacrylic acid-N,N-ethyl dimethylamide, a chain transfer agent and 1,4-dioxane to react at 60-90 DEG C in the presence of the argon to obtain polymethylacrylic acid-N,N-ethyl dimethylamide; adding the initiator, hexafluorobutyl acrylate and 1,4-dioxane, and reacting for 2-8 hours at 65-95 DEG C in the presence of argon; precipitating in n-hexane; drying to obtain the fluorine-containing high-molecular surfactant. By adopting an RAFT polymerization technology, the prepared fluorine-containing high-molecular surfactant contains a fluorine-containing unit similar to the structure of a fluorine-containing monomer, has the characteristics of narrow molecular weight distribution, adjustable structure, low critical micelle concentration, good emulsibility, low foamability and the like, and has broad application prospect in emulsion polymerization.

The invention relates to a preparation method of a nitrogen functionalized microporous carbon nanoparticle. The preparation method comprises the following steps: weighing m-phenylenediamine, terephthalaldehyde, 1,4-dioxane and 3mol/L acetum according to the mass ratio of 1: 0.6-2.5: 24-192: 1.7-6.7 and mixing uniformly; putting the mixed solution in a stainless steel reaction kettle and carrying out heat treatment at 120 DEG C for 2-4 days to obtain a nitrogen-containing polymer; and carrying out inert gas shielding in a tube furnace, heating the nitrogen-containing polymer at a heating rate of 0.5-10 DEG C/min to 700-900 DEG C for carbonization and finally naturally cooling to the room temperature to obtain the nitrogen functionalized microporous carbon nanoparticle. The prepared nitrogen functionalized microporous carbon nanoparticle has the advantages of high specific surface area, regular micropores, nitrogen functional group and spherical geometrical morphology; and when used as an electrode of a super capacitor, the nitrogen functionalized microporous carbon nanoparticle is capable of improving the high-current charging/discharging performance of the electrode while effectively keeping the high specific capacitance.

The invention discloses a method for synthesizing methyl ketone. The method comprises the following steps: adding alkyne, [(IPr)AuCl], AgOTf, a solvent, namely 1,4-dioxane and water in a reaction container, performing microwave reaction on a reaction mixture for 1h at 120 DEG C and cooling to room temperature; filtering, performing rotary evaporation to remove the solvent, and then separating by a column to obtain a target compound. The method disclosed by the invention adopts a microwave technology, and the reaction time is shortened; furthermore, the reaction only generates a byproduct, namely water, so that the reaction is in line with the requirements of green chemistry and has broad development prospects.

The present invention designs a synthesis and curing method of carborane benzo oxazine resin, and a carborane-containing benzo oxazine prepolymer has the structural formula as shown in the specification, wherein Cb is o-carborane, m-carborane or p-carborane; R is alkyl, aryl and alkylaryl. The resin is prepared by using carborane bisphenol, formaldehyde and amine as raw materials and 1, 4-dioxane as a solvent. The prepolymer can be cured by simple heating in air atmosphere. The curing process is very simple and does not require strict pollution control measures. A curing product has good thermal stability and high temperature carbon residue rate, and can be used for the study of high temperature resistant materials.

The invention relates to a method for synthesizing tetrahydroquinoline containing three continuous chiral centers through asymmetric transfer hydrogenation, wherein chiral phosphoric acid is adopted as a catalyst and substituted 1,4-dihydropyridine is adopted as a hydrogen source in the used catalysis system. The reaction can be performed under the following conditions that: the temperature is 0-70 DEG C, the solvent is 1,4-dioxane, and a ratio of the substrate to the catalyst is 20/1. According to the present invention, simple and easily-available 4-substituted-1,2,3,4-tetrahydroacridine is subjected to transfer hydrogenation to obtain the corresponding tetrahydroquinoline compound containing three continuous chiral centers, wherein the diastereoselectivity can be more than 20:1, and the enantiomeric excess can achieve 89%; and the method of the present invention has characteristics of simple and practical operation, high diastereoselectivity/enantioselectivity and high yield, and the reaction has characteristics of green atom economy and environment-protection.

The invention provides a purification method of chromatographic pure 1,4-dioxane. The method comprises the following steps of (1) eliminating 2-methyl-1,3-dioxolame impurities through hydrolysis; (2)performing adsorption: injecting the hydrolyzed 1,4-dioxane raw materials into a serially connected cation exchange resin adsorption column and active carbon adsorption column; adsorbing some aldehydes impurities in the 1,4-dioxane raw materials; (3) removing peroxides through the adsorption by a lithium aluminum hydride adsorption column; (4) performing drying and dewatering by a 4A molecular sieve; (5) performing rectification. According to the method, 1,4-dioxane industrial products with the content being 98.0 percent are used as raw materials; some adsorbable impurities can be eliminated through hydrolysis, the cation exchange resin adsorption column and the active carbon adsorption column; then, through heating treatment, the peroxides in the products are eliminated through the entering into a lithium aluminum hydride filling column. The method has the advantages that the reaction is complete; the safety is high. After the rectification, the final product content reaches 99.9 percent or higher; the moisture is less than or equal to 0.02 percent.

The invention discloses a method for preparing 1,3-diolefins. In a ternary mixed solvent of 1,4-dioxane, acetic acid and dimethyl sulphoxide, an oxidative cross-coupling reaction is carried out for ketene dithioacetals with alpha-cyano or ester and olefin which are catalyzed by divalent palladium salt in a condition with oxygen or air which is used as an oxidizing agent, in order to generate 1,3-diolefins. Compared with the reported synthetic method of 1,3-diolefins, the method has the advantages of easily available raw materials, simple operation, mild synthetic reaction condition, and high atom economy.

The invention provides a method used for preparing 1,4-dioxane from 1,3-dioxolane. According to the method, raw material gas containing 1,3-dioxolane and carrier gas is delivered into a reactor filled with a solid acid catalyst, and reaction is carried out at a reaction temperature of 120 to 160 DEG C, under a reaction pressure of 0.1 to 2.0MPa, and with gaseous hourly space velocity of 500 to 4500/h so as to obtain 1,4-dioxane, wherein partial pressure ratio of the carrier gas to 1,3-dioxolane in the raw material gas ranges from 1.0 to 50. The method is capable of realizing production of 1,4-dioxane under gas-solid reaction conditions; reaction conditions are mild; and separation of products from the catalyst is simple.

The invention provides a novel anti-tumor drug which is represented by the molecular formula (I) and specifically relates to anti-tumor 2-amino nicotinonitrile. The invention further provides a synthetic method of the anti-tumor drug. The method includes dissolving 2mmol of vanillic aldehyde or 2mmol of syringaldehyde, 2mmol of acetophenone and 2mmol of malononitrile in 1, 4-dioxane, then adding 4mmol of ammonium acetate, heating a mixture at the temperature of 120 DEG C for reaction for 20 minutes by using a microwave with the length of 300W as an assistant, adding ice water to the reaction mixture to separate out a product, and finally subjecting the mixture to recrystallization to obtain the 2-amino nicotinonitrile. The synthetic method of the anti-tumor drug is simple, and the anti-tumor drug can be rapidly and efficiently synthesized by means of a one-pot four-component reaction assisted by the microwave. The anti-tumor drug which is represented by the molecular formula (I) is capable of obviously inhibiting activities of proliferation of liver cancer cells, gastric cancer cells, breast cancer cells, pancreatic cancer cells, brain cancer cells, lung cancer cells and ovarian cancer cells.

The invention provides a method for preparing anhydrous high-purity 1, 4-dioxane from glycol dimethyl ether through one step. Through the method, high-purity 1, 4-dioxane is prepared from the glycol dimethyl ether raw material at a low temperature at a high conversion rate. In the whole reaction process, water does not react and product water is not produced so that 1, 4-dioxane-containing industrial wastewater is prevented thoroughly. The glycol dimethyl ether raw material has a high conversion ratio at a low temperature, catalyst stability is good, product 1, 4-dioxane selectivity is high and the whole process is simple and environmentally friendly.

The invention discloses a method for synthesizing alpha-alkyl ketone. The method comprises the following steps: adding alkyne, [(IPr)AuCl], AgOTf, 1,4-dioxane and water in a reaction container, performing microwave reaction on a reaction mixture for 1h at 120 DEG C and cooling to room temperature; further adding [Cp*IrCl2]2, alkali and alcohol into the reaction mixture, performing microwave reaction on the reaction mixture for 2h at 130 DEG C and cooling to room temperature; filtering, performing rotary evaporation to remove a solvent, and then separating by a column to obtain a target compound. The method disclosed by the invention is started from chemical raw materials which are easy to obtain, namely alkyne, water and alcohol, alpha-alkyl ketone is obtained under the participation of gold and iridium catalysts, and the reaction only generates water as a byproduct. Therefore, the reaction is in line with the requirements of green chemistry and has broad development prospects.

The invention discloses a method for synthesizing 1,4-dioxane by reacting 2-chlorine-ethoxyethanol with a caustic alkali such as the low-concentration solution of the hydroxide of an alkali metal or an alkaline-earth metal. The molecular ratio of the 2-chlorine-ethoxyethanol to the hydroxide of the alkali metal or the alkaline-earth metal is 1.10-1.40:1; and the mass fraction of hydroxide aqueoussolution is 5 to 25 percent. The method comprises the following steps of: adding the 2-chlorine-ethoxyethanol into a stainless steel stirred reactor; controlling the reaction temperature to be between 85 and 190 DEG C and the reaction time to be 1 to 4 hours; rectifying obtained reaction solution; collecting azeotropic distillate of the 1,4-dioxane and water; adding an entrainer; separating water; and obtaining a 1,4-dioxane product of which the purity is over 98 percent. The method solves the problems of storage and transportation difficulties of ethylene oxide, corrosion caused by strong acidic catalyst, more byproducts and the like in a 1,4-dioxane process which takes an ethylene oxide gas as a raw material, so that the production of the 1,4-dioxane gets rid of the dependence on ethylene oxide and the like; and production cost is reduced.

The invention relates to a preparation method of a zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate and a preparation method of a zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate injection. The preparation method of the zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate comprises the following steps of weighing hydroxypropyl-beta-cyclodextrin of which the weight is 4-7 times the weight of zingiber corallinum hance essential oil, dissolving zingiber corallinum hance essential oil into absolute methanol or absolute DMF or absolute 1,4-dioxane to obtain a zingiber corallinum hance essential oil solution, mixing the zingiber corallinum hance essential oil solution and the hydroxypropyl-beta-cyclodextrin solution by stirring, carrying out stirring clathration in a water-bath having a temperature of 40 to 80 DEG C for 2 to 20 hours, cooling to a room temperature, and filtering by a filter membrane to obtain a zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate aqueous solution. The preparation method of the zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate injection comprises the following step of diluting the zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate aqueous solution by injection water into the zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate injection having a required concentration. The zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate and the zingiber corallinum hance essential oil/hydroxypropyl-beta-cyclodextrin clathrate injection avoid volatilization and oxidation deterioration of zingiber corallinum hance essential oil, and can stabilize zingiber corallinum hance essential oil content.

The invention belongs to the field of pharmaceutical chemistry and specifically relates to a recrystallization method of rabeprazole sodium. A mixed solvent of a ketone organic solvent and a cyclic ether organic solvent is used for crystallization, wherein the ketone organic solvent is preferably selected from acetone, methyl ethyl ketone and cyclohexanone; and the cyclic ether organic solvent is preferably selected from tetrahydrofuran and 1,4-dioxane. The rabeprazole sodium prepared according to the method has high purity, contains less impurities and accords with crude drug standards.

A new method of synthesizing 2,4-di-substituted benzothiazole is disclosed, wherein R and R' both can be aryl groups, alkyl groups and heterocyclic ring groups. The method includes the steps of mixing a substituted thioamide substrate and a fluorine-containing alkali with a reaction solvent 1,4-dioxane, adding a known benzyne precursor slowly into the reaction solution to prepare 2,4-di-substituted benzothiazole, and performing column chromatographic purification to obtain a finish product of which the yield is 75%. The new method is low in raw material cost and the raw material is easy to obtain. The new method is simple in operation, is less in synthetic steps, is high in yield and has important application value in the fields of pharmaceutical chemistry and organic synthesis.

A synthetic method of 1,4-dioxane-2,5-diol is characterized in that concrete preparation comprises the following steps of: (1) feeding; (2) reacting; (3) post-processing; (4) preparation of the product. The invention has following advantages: 1, raw materials adopted in the invention are easily available and are cheap in price; the raw materials are all commercial raw materials or raw materials which are easy to prepare, and can satisfy the requirement of large scale production; 2, by the adoption of a simple hydrolysis reaction and simultaneously a batch charging method, the solvent amount is less, the energy and post-processing time are saved, the operation is simple, the synthetic method is suitable for large scale industrial production; 3, the condition of chemical reactions adopted in the invention is mild; there is no high temperature or low temperature reaction during the whole reaction process; during the production process, the technology is reasonable, the production is safe and reliable, and the cost is low; there is no environmental pollution; the synthetic method is suitable for large scale industrial production.

The invention provides a method for regenerating waste oil by extracting a novel combination solvent, which comprises the following steps: 1)taking waste oil and placing in a container, performing settlement in a thermotank, drying, taking a supernatant oil; 2)adding an organic solvent in the supernatant oil after filtering in the step 1), wherein the organic solvent is composed of a solvent a and a solvent b, a is one, two or three of benzene, toluene and xylene; b is one or two of tetrahydrofuran and 1,4-dioxane; and 3)extracting and refining to obtain an oil-containing mixture, sending to the thermotank for settlement, and taking the supernatant oil for distillation to obtain the reclaimed oil. In the invention, while extracting and refining, the solvent has good extracting effect to the waste oil. The experiment result displays that the regeneration method of the waste oil has the advantages of high yield and good reclaimed oil quality. In addition, the regeneration method comprises the characteristics of simple operation, mild technology condition, cycle use of the solvent, low cost and high economic benefit.

The invention discloses a preparation method of a high-sterically-hindered arylborate compound. The preparation method includes following steps: in the presence of a catalyst of a catalyst tri(dibenzalacetone)dipalladium with a phosphine ligand (wherein the phosphine ligand is 3-diphenylphosphine-2-(2,6-dimethoxylphenyl)-N-methylindole), adding an aryl chloride, bis(neopentyl glycolato)diboron, and an additive ceseium acetate to a 1,4-dioxane solution; and carrying out a reaction at 100-130 DEG C for 12-48 hours to obtain the arylborate compound. In the invention, the employed substrate is stable, is low in cost and is easy to obtain and the catalyst is unique, is easy to prepare and is suitable for the reaction of the high-sterically-hindered aryl chloride. The system is compatible of existences of functional groups, such as an ester group, an aldehyde group, methoxyl and the like so that range of the substrate is greatly developed. The catalyst system is stable, is high in catalytic activity, is wide in suitable scope, is good in selectivity and is mild in reaction conditions. The high-sterically-hindered arylborate compound can be widely applied in cross coupling reaction catalyzed by transition metal, thereby preparing various compounds, such as biaromatic hydrocarbons. The preparation method has a great application potential in synthesis of natural medicines and drug intermediates.