55 results about "Diethyl azodicarboxylate" patented technology

The invention discloses a method for synthesizing enantiomorphous pure symmetric trans-dialkyl cyclohexylamine, belonging to the field of chemistry. The method comprises the following steps of: carrying out an airtight or reflux reaction on cyclohexene oxide and an aqueous solution of alkylamine for reacting at 80-120 DEG C for 1.5-5h to obtain 2-alkyl-amino cyclohexanol, dropwise adding DEAD (Diethyl Azodicarboxylate) or DIAD (Diisopropyl Azodicarboxylate) to triphenylphosphine, 2-alkyl-amino cyclohexanol and a solvent under an ice bath for reacting for 5-20h at room temperature to obtain N-alkyl-7-azabicyclo[4, 1, 0]heptane, adding a catalyst to the N-alkyl-7-azabicyclo[4, 1, 0]heptane and the aqueous solution of alkylamine at 100-120 DEG C to carry out the airtight or reflux reaction to obtain trans-N,N'-dialkyl-1,2 cyclohexanamine, dissolving the trans-N,N'-dialkyl-1,2 cyclohexanamine in an alcoholic solvent, and adding a tartaric acid type resolving agent with the equivalent weight of 0.5 to the alcoholic solvent to resolve so as to obtain the enantiomorphous pure symmetric trans-dialkyl cyclohexylamine.

The invention discloses a synthesis method of diethyl azodicarboxylate. The synthesis method comprises the following steps that (1) under the effect of sodium ethoxide, diethyl carbonate and ethyl carbazate are heated for reaction for 1 to 6 hours, the pH of solution is regulated to 3 to 8, white crystals are separated out, the recrystallization is carried out, and hydrogenated diethyl azodicarboxylate is obtained; and (2) the hydrogenated diethyl azodicarboxylate is added at minus 15 DEG C to 45 DEG C, in the acid solution, bromine or hydrobromic acid or sodium bromide and potassium bromide are used as catalysts, excessive hydrogen peroxide is dripped, the reaction is carried out for 1 to 10 hours, the extraction is carried out, organic solvents are removed through distillation, and saffron diethyl azodicarboxylate is obtained. The invention also provides a hydrogenated diethyl azodicarboxylate intermediate and a synthesis method of the hydrogenated diethyl azodicarboxylate intermediate. The synthesis method has the advantages that diethyl carbonate is used as raw materials, cleanness and environment protection are realized, no pollution exists, raw materials can be cyclically utilized, the economy is better, the operation is simple, the reaction temperature range is wide, the reaction is stable, the energy consumption is low, the yield is high, and the industrial production is favorably realized.

The invention discloses a method for synthesizing a prucalopride midbody 4-amino-5-chloro-2,3-dihydro benzofuran-7-carboxylic acid. The method comprises the following steps: firstly, adding methyl 4-(acetyl amino)-2-hydroxy-3-(2-hydroxy ethyl) benzoate into an organic solvent, adding triphenylphosphine and azo dioctyl phthalate diethyl ester, performing cyclization to obtain a methyl 4-acetamido-2,3-dihydro benzofuran-7-formate rough product, directly chloridizing the rough product by using N-chloro succinimide to obtain a rough product methyl 4-acetamide amino-5-chloro-7-benzofuran formate, and performing hydrolysis and purification to obtain a 4-amino-5-chloro-2,3-dihydro benzofuran-7-carboxylic acid pure product. Compared with a conventional method, the method simplifies the industrial production difficulty and remarkably improves the yield, so that the method disclosed by the invention is easy in industrial production operation, nearly no organic and inorganic waste solvents are used, the total yield is relatively high, and the industrial on-scale production is facilitated.

The invention discloses a novel method for preparing a ferrocenyl polymer from controllable type polyacrylonitrile resin. The reaction of the novel method comprises the following steps of (1) preparing the polyacrylonitrile resin into a reaction system of polyvinyl tetrazolium (PVT) through a nitrile based click chemistry reaction, and enabling polyacrylonitrile, sodium azide, a catalyst and a solvent to be subjected to a reaction at certain temperature for a certain time so as to obtain an intermediate product PVT; and (2) preparing a reaction system of the ferrocenyl polymer (PVT-FeC) through a Mitsunobu reaction, and enabling the intermediate product PVT prepared in the step (1), ferrocenemethanol, triphenylphosphonium and diethyl azodicarboxylate to be subjected to a reaction at appropriate temperature for a certain time so as to obtain the ferrocenyl polymer. The molecular weight of the obtained polymer can be conveniently designed, besides, the end group of the polymer can still have activity, and the polymer can be used for synthesizing some other functional copolymers with a topological structure.

The invention discloses a composite foaming agent for a rigid PVC foam material. The foaming agent comprises the following raw materials, by weight: 5-10 parts of azodicarbonamide, 2-4 parts of diethyl azodicarboxylate, 2-3 parts of OBSH, 0.5-1.5 parts of lauryl sodium sulfate, 1-2 parts of sodium bicarbonate, 1-2 parts of zinc carbonate, 1-3 parts of urea, 0.5-0.8 part of lead stearate, 2-4 parts of citric acid, and 15-20 parts of glycol propyl ether. According to the invention, raw materials including urea, zinc carbonate, sodium bicarbonate, sodium dodecyl sulfate are adopted for modification of azodicarbonamide to prepare the composite foaming agent for rigid PVC foam material; and the composite foaming agent has advantages of decomposition temperature within the range of molding processing of rigid PVC foam material, basically balanced heat absorption-release, smooth decomposition rate, large deflating amount and no abruptness. The rigid PVC material prepared from the composite foaming agent has good mechanical properties, uniform and fine pores, thin pore wall, easily controlled processing conditions, and no emergence of burning.

The invention discloses an organic silicon pressure sensitive adhesive which is prepared by reacting the following substances in percentage by mass: 45-50% of organic silicon adhesive, 2-4% of hydroxyl polysiloxane, 2-5% of stannous octoate, 2-3% of isopropyl tri(dodecylbenzene phenylsulfonyl) titanate, 0.5-5% of alkynol, 15-30% of tackifying resin and 15-25% of azo-compound foaming agent, wherein the azo-compound foaming agent is any one of azodicarbonamide, azodiisobutyronitrile, azo-dioctyl phthalate diisopropyl ester, azo-dioctyl phthalate diethyl ester, diazo-aminobenzene or azo-dibarium formate; the hydroxyl polysiloxane is alpha,omega-dyhydroxy polysiloxane; the tackifying resin is a MQ resin. The structural size of the micro pore structure of the organic silicon adhesive can be adjusted, the micro pores can be arranged densely or sparsely, and the problem that the conventional organic silicon adhesive is not smooth in gas discharge is solved.

The invention discloses a toughened reinforced environment-friendly flame-retardant PBT/PET (polybutylene terephthalate/polyethylene terephthalate) alloy which is composed of the following components in percentage by mass: 20-60% of PBT, 10-40% of PET, 10-25% of glass fiber, 5-15% of halogen-free flame retardant, 5-15% of nano calcium carbonate, 5-10% of elastomer, 0.5-2% of maleic anhydride, 0.1-1% of diethyl azodiformate, 1-5% of plasticizer, 0.1-1% of composite nucleating agent, 0.1-1% of composite antioxidant and 0.1-2% of lubricant. Compared with the prior art, the nano calcium carbonate subjected to surface modification pretreatment and the elastomer interact and generate grafting reaction to form the core-shell particles using the nano calcium carbonate as the core and the elastomer as the shell, and the core-shell particles are used for performing toughening modification on the PBT/PET alloy, thereby greatly enhancing the notch impact strength, rigidity, heat resistance and corrosion resistance of the alloy system and keeping excellent mechanical, chemical and electric properties; the toughened reinforced environment-friendly flame-retardant PBT/PET alloy has the advantages of favorable flowability, high gloss, no halogen, flame retardancy, high safety, low smoke, no toxicity, high efficiency and low cost, achieves the flame retardancy grade UL94V-0, and can be widely used in the fields of home appliances, electronic and electric appliances, automobile industry, mechanical equipment, textiles and the like.

The invention relates to a method for synthesizing spermidine hydrochloride. The reaction formula is shown as the following formula (I) which is described in the specification. In the formula (I), theprotective group R1 of amino in 4-amino-1-butanol of a compound 2 is one of tert-butyloxycarboryl Boc-, triphenylmethyl Trt- and p-methoxytriphenylmethyl Mmt-, and a protective group R2 of propane diamine of the compound is one of tert-butyloxycarbonyl Boc-, triphenylmethyl Trt- and p-methoxytriphenylmethyl (Mmt-). A reagent used in the Mitsunobo reaction condition is one of triphenylphosphine, di-tert-butyl azodicarboxylate, diethyl azodicarboxylate and diisopropyl azodicarboxylate. The preparation method disclosed by the invention is simple in required process condition, mild in reaction condition, capable of effectively obtaining spermidine hydrochloride, relatively short in synthesis step and relatively high in synthesis yield.

The invention discloses an antibacterial and mildew-proof PP foam board and a preparation method thereof. The antibacterial and mildew-proof PP foam board is prepared by, by weight, 72-94 parts of polypropylene, 41-63 parts of chlorothalonil, 24-46 parts of cyanoethyl cellulose, 3-6 parts of dichlorophenyl dimethyl urea, 13-19 parts of tricresyl phosphate, 17-23 parts of magnetic wave stone, 10-15 parts of glass fibers, 4-8 parts of oxidized polyethlene wax, 2-3 parts of zinc isooctanoate, 15-20 parts of opal shale, 34-48 parts of waste bauxite cement, 1-2 parts of magnesium isooctanoate, 1.5-2.5 parts of diethyl azodicarboxylate, 26-39 parts of alum dregs, 2-4 parts of oxine-copper, 12-18 parts of tributyl citrate and 4-7 parts of ammonium carbonate. The antibacterial and mildew-proof PP foam board has the advantages that the chlorothalonil and the cyanoethyl cellulose are used to modify the polypropylene, the dichlorophenyl dimethyl urea, the tricresyl phosphate, the oxine-copper, the magnetic wave stone, the opal shale and the glass fibers are added for compositing, the antibacterial and mildew-proof performance of the foam board can be increased, and the water resistance and weather resistance of the foam board can also be increased.

The invention relates to a synthetic method and application of a redox induced pH-responsive type methacrylate fluorine-containing monomer. The general formula is shown in the specification, wherein a, b, c and d are respectively independent integers. The synthetic method comprises the following steps: with organic alkali as an acid-binding agent, enabling a methacrylate monomer containing a primary amine end group to react with 2,4-dinitrobenzene sulfonyl chloride in anhydrous tetrahydrofuran so as to obtain a sulfamide monomer; and with diethyl azodicarboxylate and triphenylphosphine as catalysts, enabling the sulfamide monomer to have a Mitsunobu reaction with a fluorine alcohol monomer, separating and purifying, and assembling in an aqueous solution. A strong electron withdrawing group2,4-dinitro-benzsulfamide exists in the structure disclosed by the invention and can rapidly have a nucleophilic substitution reaction with mercapto group so as to produce a secondary amine group, and the secondary amine group is protonized under corresponding pKa, so that redox induced pH response is realized. Development of fluorine-containing small molecules is facilitated, and the developmentneed of a 19FMRI probe is met. The synthetic method disclosed by the invention is simple, and the monomer is stable in quality and high in yield. The structural formula is as shown in the specification.

The invention discloses an insulating packaging material for fresh food and a preparation method thereof. The packaging material comprises a four-layered structure which successively comprises an antibacterial layer, a shock absorbing layer, an insulating layer and a protecting layer, wherein the antibacterial layer is prepared from 1-5 parts of lysozyme, 1-3 parts of chlorogenic acid, 3-5 parts of tea polyphenol, 10-15 parts of a tourmaline powder, 3-7 parts of microcrystalline graphene and 30-50 parts of chitosan. The shock absorbing layer is prepared from 20-25 parts of a modified wheat straw powder, 20-30 parts of waste paper pulp, 10-15 parts of linen fibers, 5-10 arts of aluminum borate crystal whiskers, 4-6 parts of diethyl azobarboxylate, 30-40 parts of a vinyl-vinyl acetate copolymer and 1-2 parts of a silane coupling agent. The insulating layer is prepared from 15-25 parts of diatom ooze, 5-15 parts of sepiolite amianthine, 15-20 parts of a silicon dioxide aerogel and 30-40 parts of a silica sol. The packaging material plays roles of being antibacterial and sterilizing, buffering and absorbing shock, insulating and isolating heat, and being waterproof and dampproof simultaneously, so that the preservation time and the goods shelf supply period of fresh food are prolonged greatly.

The invention discloses a synthesis method of Lupinus luteus wighteone. The method provided by the invention toakes genistein as a raw material to undergo four-step reaction so as to obtain Lupinus luteus wighteone. In the second-step reaction of the method, isoamylene bromide, potassium carbonate, and a DMF system are employed to replace isopentenyl alcohol, diethyl azodicarboxylate, triphenylphosphine and a THF system, the cost is greatly reduced, the after-treatment is much more convenient, and the yield is enhanced from 83% to 92%. In the third-step reaction, diethyl aniline, dimethylaniline, decahydronaphthalene and other high-boiling point solvents are adopted as the solvents, and under heating reflux conditions, para Claisen rearrangement of isopentenyl is completed to replace Eu(fod)3 catalyzed rearrangement adopted by original methods, thus saving the precious metal catalyst, greatly reducing the cost, and increasing the yield from original 68% to 87%.

The invention discloses a high tensile strength cable sheath tube, which is composed of raw materials: acrylonitrile-butadiene-styrene copolymer, polyvinyl chloride, chicken feather hydrolyzed powder, sodium pentanesulfonate, stearic acid decanoate Tetraalkyl ester, γ‑aminoethylaminopropyltrimethoxysilane, diethyl azodicarboxylate, polypropylene glycol dioxirane methyl ether, nano silicon carbide, nano magnesium nitride, nano aluminum oxide , Gum Arabic, Silica. The invention also discloses the production method of the above-mentioned sheath pipe, and the produced sheath pipe has the advantage of excellent high tensile strength, and at the same time, has good flame-retardant performance.

The invention relates to a new method for synthesizing chiral pharmaceutical intermediate 3-amino tetrahydropyrane and salt thereof, in particular to a method for synthesizing racemic pharmaceutical intermediate 3-amino tetrahydropyrane and salt thereof. The method is characterized by comprising a step C of: cooling glycol 3 and triphenyl phosphorus to the temperature of below 0 DEG C in an ice bath under the protection of nitrogen; slowly dropwise adding diisopropyl azodicarboxylate or diethyl azodicarboxylate into a mixture of the glycol 3 and the triphenyl phosphorus; reacting at the temperature of between 10 and 30 DEG C after dripping until the reaction is performed completely; and concentrating and drying to obtain a white solid 4 rough product, wherein the molar ratio of the glycol to the triphenyl phosphorus to the diisopropyl azodicarboxylate or the diethyl azodicarboxylate is 1:(1-3):(1-3); the used raw materials are cheap and readily available; a synthesis route is short; all reaction intermediates and a final product are not required to be subjected to column chromatographic purification; and a large amount of R or S-type 3-amino tetrahydropyrane with high optical activity and racemate thereof can be conveniently prepared from natural L or D-type glutamic acid or racemate thereof serving as a raw material. The method has the advantages of low cost and higher efficiency; and an obtained product has high chemical purity and optical purity.

The invention discloses a method for preparing dialkyl azodicarbonic acid. The method comprises the steps of: mixing dimethyl azodicarbonic acid or diethyl azodicarbonic acid with sodium alkoxide solution, heating and reacting for 1-24h, and carrying out transesterification reaction between the dimethyl azodicarbonic acid or diethyl azodicarbonic acid and alcohol under the catalytic action of the sodium alkoxide; after the reaction is completed, regulating the pH value of the solution to 6-8, extracting an organic phase for 2-3 times with dichloromethane, combining the organic phases, drying for 8-12h with anhydrous sodium sulfate, and then performing reduced pressure distillation or recrystallization to obtain dialkyl azodicarbonic acid ROOCN=NCOOR, wherein R is alkyl containing 2-16 carbon atoms. According to the method, the dimethyl azodicarbonic acid or diethyl azodicarbonic acid is selected as raw materials, and is easily available; and the production cost is low, the economy is good, and pollution to the environment does not exist; the method for preparing the dialkyl azodicarbonic acid through esterification is simple to operate, short in process route, mild in reaction conditions, and high in yield, as well as suitable for industrialized development.

The invention relates to a synthesis method based on amination reaction of aryl siloxane. The method comprises the following steps: adding AgF, a reactant I, a reactant II, a butanone solution and a number 5 magneton into a reactor in sequence, connecting a condenser pipe, introducing condensate water from bottom to top, placing the reactor in an oil bath pan at 30-70 DEG C, heating, stirring and reacting for 10-12 hours, terminating the reaction, and purifying the product to obtain an aryl siloxane amination product, wherein the reactant I is optionally selected from phenyl triethoxy silane, p-tert-butyl phenyl triethoxy silane, p-methoxy phenyl triethoxy silane, p-methyl phenyl triethoxy silane, p-chlorphenyl triethoxy silane or 4-triethoxy silicon biphenyl; and the reactant II is diethyl azodicarboxylate. The method is mild in reaction condition, high in selectivity, relatively high in yield and environment-friendly; and the compound has certain biological activity and can be used in the field of synthesis of drugs, pesticides and paint dyes.

A foaming agent for an EPDM sponge rubber is disclosed by the invention, and consists of the following raw materials in parts by weight: 5-10 parts of 4, 4'-oxybis(benzenesulfonyl hydrazide), 4-6 parts of N,N'-dinitroso pentamethylene tetramine, 2-5 parts of diethyl azodiformate, 1-3 parts of p-toluenesulfonyl semicarbazide, 4-6 parts of ammonium bicarbonate, 2-5 parts of coconut oil monoethanolamide, 8-12 parts of ethylenediamine, 20-30 parts of propylene glycol, 2-5 parts of benzoic acid, 1-2 parts of alum, and 0.5-1.5 parts of zinc oxide. The foaming agent of the invention is excellent in foaming power, high in foaming ratio, steady in process, low in cost and convenient to use, and the generated foams has good temperature adaptability and disperse uniformity. The EPDM sponge rubber material prepared by the foaming agent is good in mechanical properties, low in density, fine in micropore and uniform in dispersion.

The present invention relates to an orlistat preparation method, which concretely comprises: dissolving (3S, 4S)-3-hexyl-4-[(R)-2-hydroxy tridecyl]-2-oxetanone, triphenyl phosphorous and N-formyl-L-leucine in tetrahydrofuran, adding diethyl azodicarboxylate in a dropwise manner under stirring, stirring overnight, taking out the organic phase, carrying out pressure reducing concentration, and carrying out silica gel column chromatography on the remaining material so as to obtain the product orlistat. The orlistat preparation method of the present invention has characteristics of simple preparation process and low production cost.