118 results about "Phosphoramide" patented technology

The present invention relates to flame retardant compositions of compatibilized polyphenylene ether-polyamide resin blends containing at least one phosphoramide compound. The present invention also relates to articles made from the resin compositions as well as methods to make flame retardant compositions of compatibilized polyphenylene ether-polyamide resin blends.

The invention discloses a diethoxy phosphorothioate organic phosphorus pesticide haptens and a method for preparing the same. The haptens are products of nucleophilic substitution of diethylthiophosphoryl chloride and phenol derivates with a carboxyl or an amine acid. The invention provides a series of haptens aiming at a common structure of the organic pesticides of diethoxy phosphorothioate. The haptens are similar to the counterparts of organic pesticides having a common structure of the diethoxy phosphorothioate in terms of molecular structure, stereochemistry and electron distribution, wherein phenol derivative arms which have carboxyls and vary in length are introduced onto the oxygen atoms of the diethoxy phosphoramide to be bound with carrier proteins. The haptens and the metod lay a technical foundation for the preparation of antibodies of diethoxy phosphorothioate organic phosphorus pesticides and the development of quickly testing products.

The invention discloses a chiral spiro phosphoramide derivative, which is a compound with a structural formula (1), a racemate or an optical isomer thereof. The chiral spiro phosphoramide derivative has a chiral spirobiindane skeleton, and is synthesized by adopting a 1,1'-spiro indane-7,7'-diphenol derivative with a spiro skeleton and a characteristics of optical activity as a chiral starting raw material. The chiral spiro phosphoramide derivative is a novel Bronsted acid organic small molecule catalyst, and can be widely used for catalysis of a plurality of asymmetric organic reactions.

The invention discloses a hyperbranched polyphosphoramidate and a preparation method thereof. The preparation method of the hyperbranched polyphosphoramidate comprises that one or more B' B2 type hydramine monomers and one or more A2 type monomers selected from phenyl dichlorophosphate, isopropyl phosphonic dichloride, ethyl dichlorophosphite and the like are heated to undergo a reaction in the presence of at least one catalyst under a nitrogen protective atmosphere; reaction products are subjected to solution polymerization to form an AB2 type monomer; and the AB2 type monomer is subjected to further polycondensation to form the hyperbranched polyphosphoramidate. The hyperbranched polyphosphoramidate has the characteristics that a skeletal structure of the prepared hyperbranched polyphosphoramidate contains phosphatide bonds and phosphamide bonds and thus the hyperbranched polyphosphoramidate has good biodegradability; reaction raw materials of the hyperbranched polyphosphoramidate have wide sources; the reaction raw materials are commercial monomers; and the hyperbranched polyphosphoramidate is prepared by typical condensation polymerization. The preparation method has the advantages of mature synthesis way, simple reaction devices, operation and separation purification processes, and high product yield. Ends of molecular chains of the prepared hyperbranched polyphosphoramidate contain a lot of function groups and thus the prepared hyperbranched polyphosphoramidate can react with multiple active groups. The hyperbranched polyphosphoramidate has a wide application prospect especially in a biological material field.

The invention relates to the field of clean energy. In order to solve the problem that existing biodiesel is poor in safety and popularization in application, the invention provides an alcohol ether biodiesel which is formed by uniformly mixing 68-92wt% of base liquid, 0.15-1.5wt% of cetane number improver, 5-8wt% of linear ether, 1.5-3wt% of surfactant, 0.03-1wt% of pour point depressant, 1.3-3.5wt% of cosolvent and 0-15wt% of degenerated methanol. The base liquid is a mixed liquor of oleyl alcohol and octanol or cocoanut oil alcohol. The mass ratio of cocoanut oil alcohol and octanol in the mixed liquor of oleyl alcohol and octanol is arbitrary. The linear ether is any one or more of linear ethers. The surfactant comprises alkanolamide. The pour point depressant comprises any one or more of an ethylene-vinyl acetate copolymer, a methyl acrylate polymer or a styrene ester polymer. The cosolvent is isobutanol or n-butanol. The degenerated methanol is formed by mixing methanol and hexamethyl phosphoramide. The alcohol ether biodiesel is high in combustion ratio, high in safety, low in manufacturing cost and convenient to widely popularize.

The invention belongs to the technical field of medicinal chemical synthesis, and particularly relates to a preparation method for 5-fluorocytosine. The preparation method comprises the following steps of: dropwise adding ethyl formate in xylene, carrying out a condensation reaction with methyl fluoroacetate under the action of a metal catalyst, and heating, stirring and carrying out heating heat preservation to obtain an intermediate; carrying out chlorination substitution on the intermediate with a chlorinating agent in the presence of an organic amine catalyst to obtain a chlorination product; carrying out ammoniation substitution on the chlorination product in an ammonia gas pressure environment and under the action of phase transfer catalysts (N-alkyl phosphoramide, methylene bridged phosphate and tetrabutylammonium bromide to obtain an ammoniation product; carrying out acidic hydrolysis on the ammoniation product to obtain 5-fluorocytosine. The 5-fluorocytosine prepared by the preparation method disclosed by the invention is high in yield and high in purity; use of highly-toxic fluorine is avoided during the preparation process, thus reducing damage and injury to equipment and operating personnel during a production process.

The invention provides a compound of formula I:wherein R1, Ra, Rb, Rc, and Rd have any of the values defined in the specification, as well as pharmaceutical compositions comprising such compounds or salts. The compounds are useful for treating cancer in animals.

The invention discloses a deoxyribonucleic acid (DNA) base analogue with a photo-crosslinking group biaziridine and a synthetic method thereof, and relates to the DNA base analogue and the synthetic method thereof. The DNA base analogue with the photo-crosslinking group biaziridine is a biaziridine phosphoramidite monomer; an intermediate product with two hydroxyl groups is connected on the basis of a compound 1; a material 1-amino-hexylene glycol is led; an amido bond is formed under condensation of dicyclohexylcarbodiimide and 1-hydroxybenzotriazole, so as to obtain an immediate product 2; the material 4-4'-dimethoxy triphenyl methyl chloride is led; pyridine and dichloromethane are taken as solvents; an immediate product 3 is obtained under catalytic action of 4-dimethylamino-pyridine; the material 2-cyanoethyl N, N-diisopropyl chlorinated phosphoramide is led; N,N-diisopropylethylamine is taken as alkali and a catalyst; dichloromethane is taken as a solvent, so as to obtain the final product under the condition of anaerobic reaction without water.

The invention relates to a preparation method for improving the flame retardance of water-based paint and adhesive by virtue of carbon nanotubes. The preparation method comprises the following steps: adding water, an emulsifier and O-methyl-O-(2-isopropoxy carboxyl phenyl) sulfo-phosphamide into a reaction container, heating and stirring for 40 minutes, adding a monomer A, emulsifying, heating to be 90 DEG C, dripping an initiator, reacting for 1 hour, further adding 5-carboxyl amyl-triphenyl phosphorus bromide and 6-maleimide hexanoic acid, and stirring and reacting for 2 hours, thereby obtaining nuclear-layer emulsion; simultaneously dripping a monomer B and an initiator into the nuclear-layer emulsion, stirring and reacting for 40 minutes at 95 DEG C, adding a coupling agent grafted double-walled carbon nanotube solution and a crosslinking agent, reacting for 2-3 hours at 75-85 DEG C, reducing the temperature to be 50 DEG C, adding an emulsifier, reacting for 70 minutes, adding sodium hydrogen sulfite and 2,4-diamido-6-hydroxy pyrimidine, reacting for 1 hour at 80 DEG C, and adding ammonia water to adjust the pH value to be 7-8, thereby obtaining the flame-retardance water-based paint and adhesive. By adopting the preparation method, both the flame retardance of acrylate resin is greatly improved, and the defect that acrylate resin emulsion is yellowish after being formed into a film is alleviated.

The invention provides modifying organoaluminum co-catalysts for improved performance. Processes of making catalyst compositions are provided. In an exemplary embodiment, the processes include modifying an organoaluminum compound with a modifier that decreases the initial reducing strength of the organoaluminum compound, where the modifier can be an ether, an anhydride, an amine, an amide, a silicate, a silyl ether, a siloxane, an ester, a carbonate, a urea, a carbamate, a sulfoxide, a sulfone, a phosphoramide, or a combination thereof. The processes further include adding a transition metal complex to the mixture of the organoaluminum compound and the modifier; and obtaining a catalyst composition including the organoaluminum compound and the transition metal complex.

The invention relates to a phosphoric acid amide bifunctional catalyst derived from cinchona alkaloid and a synthetic method thereof. According to the invention, the chiral phosphoric acid amide bifunctional catalyst with high efficiency catalytic activity provided in the invention is prepared in one step by reacting corresponding primary amine produced by ammonification of cinchona alkaloid and derivatives thereof with phosphoric acid acyl chloride. The catalyst provided in the invention has the advantages of a novel structure, stable properties, high catalytic activity, etc., and the synthetic method for the catalyst is simple.

The invention provides a modified ethylene propylene terpolymer and a preparation method. According to the invention, easily dispersed hyperbranched phosphoramide modified graphene oxide is obtained in the manner of in situ synthesis of hyperbranched phosphoramide on the surface of the graphene oxide; the modified ethylene propylene terpolymer master batch is obtained in the manner of blending the hyperbranched phosphoramide modified graphene oxide with a softener, an accelerant, a reinforcing agent and an anti-ageing agent; and the modified ethylene propylene terpolymer is obtained in the manner of blending and vulcanizing the modified ethylene propylene terpolymer master batch with a vulcanizing agent. The hyperbranched phosphoramide modified graphene oxide in the modified ethylene propylene terpolymer provided by the invention is uniformly dispersed; and the modified ethylene propylene terpolymer has higher mechanical property, flame retardant property and heat-conducting property, and the limit oxygen index can reach up to 25%. The preparation method for the modified ethylene propylene terpolymer, provided by the invention, is simple and easy to realize, is suitable for large-scale production and is beneficial to industrial popularization.

Certain cyclic phosphoramide ester compounds useful, inter alia, as halogen-free flame-retardant compounds, are disclosed. The compounds are particularly useful for providing flame retarded polyurethane foams. (I)

The invention relates to a copolymerized flame-retardant polyamide fiber and a preparation method thereof. The preparation method comprises the following steps that a flame-retardant polyamide copolymer serves as all or part of spinning raw materials for spinning to obtain the copolymerized flame-retardant polyamide fiber, wherein the flame-retardant polyamide copolymer is prepared by mixing a flame retardant salt with a polyamide 66 oligomer and / or a polyamide 6 oligomer and then carrying out condensation polymerization, the flame retardant salt is prepared from N,Ndi (6aminohexyl) phenyl phosphoramide and binary acid HOOCR1COOH through a high-temperature and high-pressure reaction, the temperature of the high temperature is 210-220 DEG C, and the pressure of the high pressure is 1.7-1.9MPa, and the main material of the finally prepared copolymerized flame-retardant polyamide fiber is the flame-retardant polyamide copolymer. The preparation method is simple to operate, the flame-retardant polyamide copolymer is excellent in flame retardance and good in spinnability, and the prepared copolymerized flame-retardant polyamide fiber is a functional fiber with flame retardance and canbetter meet the requirements of the fields of medical treatment and public health, professional clothing, clothing home textiles and the like in modern life on the flame-retardant polyamide fiber.

The invention relates to a method for preparing flame-retardant polymer polyol from phosphamide. The method mainly comprises the following steps: a, reacting phosphoryl dichloride with organic diaminein a nitrogen atmosphere, adding an acid-binding agent, reacting at 60 DEG C for 2 hours, and filtering to obtain a colorless transparent solution; and b, adding a formaldehyde solution into the phosphamide solution obtained in the step a, heating to react for a period of time, mixing the obtained solution with polyether polyol, heating to react completely, and vacuumizing to remove residual monomers to obtain the flame-retardant polymer polyol with the nitrogen content of 6-9% and the phosphorus content of 3-5% in terms of the weight of the polymer polyol. The polyurethane foam plastic prepared from the flame-retardant polymer polyol has a foaming foam oxygen index of about 30%, good flame retardancy and low smoke generation amount.

The invention discloses a method for preparing PMMA with high molecular weight and narrow molecular weight distribution. According to the method, firstly, an iodine compound is obtained by an in-situreaction of an azo initiator and an iodine simple substance, and a combined action of the generated iodine compound and a phosphoramide additive regulates and controls the reaction to obtain the PMMAwith the high molecular weight and the narrow molecular weight distribution. The reaction is mild in condition, is simple to operate, and is high in utilization rate of raw materials; and the conversion rate of converting elemental iodine into the iodine compound is 98% or above, the monomer conversion rate is in a range of 80-98%, the number average molecular weight of the prepared poly(methyl methacrylate) is between 30000 and 120000, the weight average molecular weight is between 37000 and 170000, and the molecular weight is distributed in the range of 1.2-1.6.

The invention discloses a high-strength solid buoyancy material used in deep sea and a preparation method of the high-strength solid buoyancy material. The high-strength solid buoyancy material comprises the following components in parts by mass: 10-30 parts of epoxy resin, 1-3 parts of an anti-impact agent, 3-5 parts of a curing agent, 4-6 parts of a solvent, 5-15 parts of hexamethyl phosphoramide, 6-8 parts of a catalyst, 5-15 parts of hollow glass beads, 10-20 parts of inorganic packing, 6-8 parts of calcium stearate, 4-8 parts of aluminum oxide, 15-25 parts of a toughening agent, 10-12 parts of an amino silane coupling agent and 2-4 parts of a diluent. The high-strength solid buoyancy material has the advantages of being small in number of steps, low in cost and simple in process, in addition, the dispersibility and the compatibility of the hollow glass beads in an epoxy substrate can be improved through grafting modification, and furthermore, epoxy groups of a polymer base are cured with the epoxy resin substrate, so that the strength of the prepared solid buoyancy material can be high, the use depth of the prepared solid buoyancy material can be up to 7000-10000m, and requirements of ocean development and seabed exploration can be met.

The invention discloses a method for synthesizing nucleoside triphosphate and nucleoside diphosphate from an all-protected nucleoside phosphoramidite intermediate through acid catalysis. The method comprises the following steps of: generating a phosphoramidite intermediate crude product under an alkaline condition by taking carbobenzoxy protected nucleoside and benzyloxydiisopropylamino phosphorochloridite as raw materials, subjecting the phosphoramidite intermediate crude product to weak acid catalytic hydrolysis to obtain a nucleoside- H-phosphonate intermediate crude product, subjecting the nucleoside-H-phosphonate intermediate crude product and alkylamine to oxidative coupling, carrying out column chromatography on the resulting product to obtain an all-protected nucleoside phosphoramidite precursor, subjecting the nucleoside phosphoramidite precursor to catalysis and hydrogenation in an N-N-dimethylfomamide solution to remove all protective groups, filtering the resulting product to remove palladium on an activated carbon, and reacting the resulting product with pyrophosphate or monophosphoric acid alkyl ammonium salt under a condition in the presence of a weak acid catalyst to obtain a nucleoside triphosphate product and a nucleoside diphosphate product. By adopting the method disclosed by the invention, reaction velocity and yield of the pyrophosphoric acid and monophosphoric acid reagents with the phosphoramidite intermediate are greatly improved, and an efficient, universal and novel method for the chemical synthesis of the nucleoside 5'- triphosphate and the nucleoside 5'-diphosphate is established.

The invention relates to a synthetic method of p-flurobenzaldehyde, which belongs to the chemical and pharmaceutical field. In the synthetic method, the p-chlorobenzaldehyde and potassium fluoride react under the condition of a solvent and a catalyst at high temperature, wherein, the solvent is one of sulfolane, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, hexamethyl phosphoramide, nitrobenzene and ortho-nitrotoluene; the catalyst is one of or the mixture of two or more than two of benzyl triethyl amine chloride, tetrabutylammonium bromide, hexadecyltrimethylammonium chloride, methyltrioctylammonium chloride, tetraphenylphosphonium bromide, methyltriphenylphosphonium bromide, benzyl triphenyl phosphonium bromide and polyethylene glycol dimethyl ether. Compared with the conventional preparation method, the synthetic method of the invention has the advantages of cheap raw materials, short synthetic route and little 'three wastes' discharge. As the amount of the catalyst used is reduced and the price of the solvent is low, the production cost of the p-flurobenzaldehyde is decreased.

The invention discloses a high-strength fly ash brick and a preparation method thereof, and belongs to the technical field of building material preparation, the preparation method of the fly ash brick comprises the following steps: 1, mixing and stirring fly ash, gypsum, calcium carbonate, calcium chloride and potassium sulfate to obtain a mixture; mixing and stirring the mixture with a reinforcing agent, cement and zeolite in parts by weight, and adding water in the stirring process to obtain a mixed material; and 2, carrying out digestion treatment on the mixed material; carrying out compression molding treatment to obtain a green body, transferring the obtained green body into a still kettle, and curing for 12 hours to obtain the high-strength fly ash brick. The reinforcing agent in raw materials of the fly ash brick takes brucite fiber as a matrix, the surface of the brucite fiber is coated with a layer of polyphosphoric acid, the polyphosphoric acid and a flame-retardant component are combined in an ionic bond or coordination form, the flame-retardant component is introduced into the surface of the brucite fiber to form a polyphosphamide coating layer, the mechanical property is improved by adding the reinforcing agent, and the flame retardant property is improved.

The invention relates to a spinning sewage environmental-protection treating agent, which is composed of the following ingredients: amino trimethylene phosphonic acid, pyrrolidine, starch xanthate, NPAM, copper chloride dehydrate, peracetic acid, boric acid, sodium formate, sodium hydrosulfite, sodium hypochlorite, DL-methionine, sodium citrate, white carbon black, caustic alkali, sodium aluminate, flyash, diatomite, activated carbon, hexamethyl phosphoramide, lemon essential oil, propylene glycol, acetic ether, ethylene oxide, triethanolamine, polymethyl hydrogen siloxane, polyethylene glycol octylphenol ether, poly(diallyldimethylammonium chloride), starch phosphate, 2-ethylhexyl acrylate, butyl hydroxyanisole and deionized water. The product has fast reaction speed, and no toxic or harmful gas is generated during the process. A product obtained after the reaction is stable and will no longer be decomposed into toxic substances. The spinning sewage environmental-protection treating agent is efficient and nontoxic, is safe to human before and after the reaction, is noncorrosive to objects, and has high sewage treatment efficiency.

New phosphoramide derivatives of formula (I) and the salts and solvates thereof, wherein the meanings of the various substituents are as disclosed in the description. Said compounds are useful as antiinflammatory and analgesic agents.

The invention provides a sulfur-containing silane synthesizing method. According to the synthesizing method, one or several of dimethyl formamide, dimethyl acetamide, hexamethyl phosphoramide and 1,3-dimethyl-2-imidazolidone is utilized as a solvent; sodium and sulfur are pretreated in the solvent to obtain sodium suspension liquid and sulfur suspension liquid; the sodium suspension liquid is added into the sulfur suspension liquid to react to obtain sodium polysulfide; halogenated alkyl alkoxy silane is added into the sodium polysulfide to react and be decontaminated to obtain a sulfur-containing silane finished product. According to the synthesizing method disclosed by the invention, sulfur-containing silane is synthesized in the solvent, so that not only is reaction efficiency in production improved, but also impurity introduction in a production process is avoided, quality of a final product is guaranteed, and purity, yield and calculation yield of the final product are improved; meanwhile, potential safety hazards and environmental pollution in a sodium and sulfur treating process are avoided, and environment-friendly treating cost in the production process is reduced.

The invention discloses an electrochemistry sensor for measuring organophosphorus pesticide residues and measurement method thereof. The surface of the electrochemistry sensor is decorated with gold nanoparticles, the sulfydryl methylacetamide phosphoramide molecules are automatically assembled and connected with the gold nanoparticle surface through an Au-S key. Based on the principle that acetylcholin esterase can have strong interactions with organophosphorus, the electrochemistry sensor provides an electrochemistry measuring method that requires no enzyme catalysis. The sensor uses short measurement time, can be used for single and gross measurements of organophosphorus.

The invention discloses a lithium-based anti-bacteria metal surface treatment agent which comprises the following components in parts by weight: 15-20 parts of polyvinyl alcohol, 0.4-0.5 part of tea saponin, 3-4 parts of lithium lubricating grease, 0.4-1 part of ferrocenecarboxylic acid, 0.1-0.2 part of hexahydrophthalic anhydride, 0.1-0.12 part of DBNPA, 0.5-1 part of potassium sorbate, 0.1-0.2 part of hexamethyl phosphoramide, 1-2 parts of sodium bisulfite, 6-8 parts of sericin, 0.08-0.1 part of boric acid, 10-20 parts of methylbenzotriazole and 180-200 parts of deionized water. According to the invention, water-soluble polymer polyvinyl alcohol and sericin are mixed, and through modification of boric acid, tensile strength and heat stability of a blended membrane are improved, the membrane adsorbed on the surface of the metal is more uniform and stable since corrosion inhibition alkali liquor using methylbenzotriazole as a main material is added, the metal material is protected from being corroded by harmful media in atmosphere and water, a better corrosion inhibition effect is achieved, and bacterial and fungal contamination can be effectively resisted sine the added DBNPA, potassium sorbate and other various metal surface treatment agent additives are compatible.

The invention provides a cyclophosphamide synthetic method. The cyclophosphamide synthetic method is characterized by comprising the following steps: adding dichloroethane into a reaction flask; slowly adding phosphorus oxychloride; starting to drip a 3-amino propanol and triethylamine mixed solvent; performing a reaction after finish of dripping to prepare a 2-chloro-2-oxo-[1,3,2] oxaphosphorinane solution; then transferring the 2-chloro-2-oxo-[1,3,2] oxaphosphorinane solution into the pressure reaction flask; adding triethylamine; controlling the temperature; continuously pumping into ammonia gas; keeping a certain pressure for a reaction; separating an organic phase from a reaction liquid; performing vacuum concentration on the organic phase till the organic phase is dry; adding a solvent; and performing crystallization to obtain cyclophosphamide. The cyclophosphamide synthetic method is high in yield, less in byproduct, simple in step and convenient to operate and facilitates industrial production.

The invention provides a cyclohexanediamine-derived phosphamide chiral ligand as well as a preparation method thereof and an application thereof. The method comprises the following steps of: first, protecting one amino of chiral source cyclohexanediamine by using phthalic anhydride; and after the chiral source cyclohexanediamine is acylated with dialkyl phosphoryl chloride, removing a protecting group by using hydrazine hydrate; and performing N-alkylation reaction on the chiral source cyclohexanediamine and halohydrocarbon, so as to obtain the phosphamide chiral ligand. According to the invention, the phosphamide chiral ligand can be used for catalyzing asymmetric addition reaction of zinc alkyl and a carbonyl compound; the yield of an addition product is high up to 99 %; and the enanitomer selectivity ee value is high up to 96 %.

The invention relates to a continuous preparation method and a preparation device of N-n-butyl thiophosphoric triamide. The preparation method comprises the following steps: (1) adding a thiophosphoryl chloride toluene solution and n-butylamine into a micro-channel reactor for substitution reaction to obtain an N-n-butyl dichloro thioxophosphamide toluene solution, treating the N-n-butyl dichlorothioxophosphamide toluene solution with an anion exchange resin, and feeding the treated N-n-butyl dichloro thioxophosphamide toluene solution into a storage tank; (2) adding the solution in the storage tank and ammonia gas into a tubular reactor for reaction to obtain an N-n-butyl thiophosphoric triamide toluene solution; and (3) carrying out extraction washing, organic phase concentration recrystallization, separation and drying on the obtained solution to obtain the high-purity N-n-butyl thiophosphoric triamide. According to the continuous preparation method and the preparation device disclosed by the invention, the continuity of the production process of the N-n-butyl thiophosphoric triamide is realized, the defect of intermittent operation of a kettle type reactor is avoided, the process is simplified, the reaction selectivity is improved, and the purposes of clean production, shortening of the production period and reduction of the production cost are achieved.

Compounds of Formula I: I and their pharmaceutically acceptable salts are useful for the inhibition of HIV reverse transcriptase. The compounds may also be useful for the prophylaxis or treatment of infection by HV and in the prophylaxis, delay in the onset or progression, and treatment of AIDS. The compounds and their salts can be employed as ingredients in pharmaceutical compositions, optionally in combination with other antiviral agents, immunomodulators, antibiotics or vaccines.

The invention discloses a dihydropyrimidine-phosphoramide derivative, and a preparation method and an application thereof. The above compound has a structure represented by formula I. The invention also relates to the preparation method of the compound represented by formula I, a medicinal composition containing the compound, and the application of the compound in the preparation of anti-HBV drugs.