251 results about "Triethylphosphite" patented technology

The invention provides a group of polyhydroxy stilbene compounds, their preparing process and use for suppressing and eradicating SARS coronavirus. The preparing process comprises, preparing phosphonic ester by reacting multi-alkyl substituted chloro (bromo) methoxyl or pyridine compounds with triethyl phosphate, then reacting phosphonate ester compound with multi-alkyl (oxy) phenylpyridine methyl aldehyde to obtain multi-alkyl (oxy) stilbene compounds. Finally acting with boron tribromide to obtain polyhydroxy stilbene compounds with substituent groups.

The invention discloses a preparation method of 4-acetoxyl-2-methyl-2-butylenoic aldehyde. In the traditional method, the yield is lower, the waste water amount is larger, and the requirements on equipment are higher. The preparation method comprises the following steps of: reacting 2-halogenated ethanol as a raw material with an acylating agent to obtain halogenated ester; then preparing phosphonate ester through the Arbuzov reaction between the halogenated ester and triethyl phosphite; preparing glutaraldehyde acetal through the Wittig-Horner reaction between the phosphonate ester and 1,1-dimethoxy acetone under the action of alkaline, and carrying out deprotection on the glutaraldehyde acetal under the acidic condition to obtain glutaraldehyde, namely, the 4-acetoxyl-2-methyl-2-butylenoic aldehyde. The invention has less three waste generation, good reaction selectivity, less by-products and higher yield.

The invention relates to a method for preparing imatinib, which comprises the following steps of: with a compound N-(5-Amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidineamine shown as the structural formula (II) and a compound 4-[(4-Methylpiperazin-l-yl)methyl]benzoic acid shown as the structural formula (III) as initial raw materials, dropwise adding phosphite ester at 50-90 DEG C for 1-2 hours inthe presence of a catalyst in an organic solvent; and continuously insulating and reacting at 50-90 DEG C to obtain the compound imatinib shown as the structural formula (I). The organic solvent is N,N-dimethylformamide, N,N-dimethylacetylamide or N-methylpyrrolidone. The catalyst is pyridine; and the phosphite ester is trimethyl phosphate, triethyl phosphate or triphenyl phosphate. The technical scheme of the invention has the advantages of simple reaction step, easy control of reaction, short production cycle, low toxicity of used raw materials, less pollution to the environment and higher product quality, and the yield can reach 95 percent, and the purity reaches 99.5 percent.

The invention relates to a kind of ligustrazine derivant, preparation method and medicinal compound and its application, belonging to chuanxiong rhizome derivant medicine technique. The structure general formula is as that: Ar is hydroxybenzene, fluorophenyl, chlorphenyl, methylbenzene, methoxybenzene, nitrobenzene, cyanobenzene, furan group, ligustrazine or thiofuran. Said preparation method comprises following steps: mixing intermediate 2- chloromethyl- 3, 5, 6- trimethyl pyrazine and halogenated benzyl, triethyl phosphite; heating and refluxing, adding waterless tetrahydrofuran and NaH at tetrahydrofuran bath condition, dropping mixing solution of aromatic aldchyde and waterless tetrahydrofuran, stirring, extracting, drying, filtering, steaming to remove disslovant, separating residues with fast column chromatography, recrystallizing with methanol, and getting ligustrazine derivant. Said product and medical findings can be used to produce medicinal compound, and medicine for preventing angiocardiopathy and cerebrovascular diseases such as ischemic disease, atherosclerosis and coronary disease.

The invention relates to a production method of triethyl phosphite, which belongs to the technical field of chemical production. Absolute ethyl alcohol, phosphorous trichloride are taken as main material, pure benzol is taken as solvent, triethylamine is taken as acid-binding agent, liquid ammonia is taken as reducing agent, and the triethyl phosphate is prepared through the processes of three-complex liquor preparing, synthetic reaction, water scrubbing reaction, layering, drying, crude distillation, rectifying, recovering and ammonia recovery and the like. The method adopts continuous production process of triethylamine, the material charging and the product discharging are continuous, the production capacity is strong, and the product quality is stable. With equal equipment and investment, the capacity of the method can be 6 to 7 times as the capacity of intermittent method. The method solves the problems of the prior production method that the production capacity is small, the production cycle of the product is long, the material consumption is large, the quality is unstable, the discharge amount of 'three wastes' is large, and the yield can not be guaranteed. The method has the advantages that the liquid ammonia is taken as reducing agent, the cost is low, the recovery factor of excess ammonia can reach more than 90 percent, the recovered ammonium chloride can be used as the crude product of ammonium fertilizer, the production cost is lowered, and the environmental pollution is reduced.

The invention discloses a new technology for synthesizing AE-active ester with accelerant, which is made by condensation reaction in the triethyl phosphate and triethylamine solvent. The invention is characterized by the following: introducing pyridine with high hydroscopicity as the accelerant in order to accelerate the reaction proceeding according to the forward direction based on the original technology; changing the reaction solvent system (the mixed solvent which is comprised by acetonitrile and carrene according to (0.9-1.0):1); avoiding the problem of water content which is introduced by the new solvent; improving the normal reaction temperature; reducing the operation difficult; reducing the strength; improving the product efficient to more than 92%. The invention also achieves the recycling of the solvent by distillation.

The invention discloses a method for synthesizing AE-active ester. The AE-active ester is prepared by taking aminothiazoly loximate and dithio-bisbenzothiazole as raw materials and carrying out condensation reaction in the presence of triethylamine and triethyl-phosphite. The method is characterized in that higher fatty acid with diffusion effect is introduced into the condensation reaction and a mixed solvent consisting of methylene dichloride and acetonitrile is adopted, wherein the volume ratio of the methylene dichloride to the acetonitrile is (1.2-1.6):1. On the basis of the traditional process, the invention introduces a dispersion agent with diffusion effect, overcomes the defects of unstable structure and short preservation time of the AE-active ester, ensures that products are easy to preserve, changes a reaction solvent system and improves the yield up to over 91 percent. In addition, the solvent can be recycled so as to reduce the production cost and has higher implementation benefit and economic benefit.

The invention discloses a synthesis method for resveratrol, including (1) discharging hydrogen bromide gas to benzene solution of p-methoxy benzyl alcohol to obtain p-methoxy benzyl bromide, (2) carrying out reaction of p-benzyl bromide with triethyl phosphate to obtain diethyl p-methoxy benzyl phosphate, (3) carrying out reaction of diethyl p-methoxy benzyl phosphate with sodium amide and 3,5-dimethoxybenzaldehyde to obtain (E)-3, 4', 5-trimethoxystilbene, and (4) carrying out reaction of (E)-3, 4', 5- trimethoxystilbene with aluminum iodide to obtain the final product. The invention has the advantages of raw materials easy to get, lowered cost, mild reaction conditions, simplified operation, and enhanced yield.

The invention relates to a synthetic method of an alpha-hydroxyl carbonyl compound. The method is as below: mixing a carbonyl compound (I) with an organic phosphorus compound in an organic solvent; adding a catalyst cesium carbonate; and reacting under aerobic conditions to obtain the alpha-hydroxyl carbonyl compound (II). R1 is selected from the group consisting of hydrogen, alkyl, alkoxy, amino, aromatic base, substituted aromatic base and heterocyclic aromatic base; R2 is selected from alkyl, carbonyl, ester and phenyl; R3 is selected from alkyl, carbonyl, ester group and phenyl. Or, R1 combines with R2 to form naphthenic group or substituted cycloalkyl, benzo cycloalkyl base or substituted benzo cycloalkyl base, indole ring or substituted indole ring. Or, R2 combines with R3 to form the cycloalkyl or substituted cycloalkyl. The organic phosphorus compound is triphenylphosphine or triethyl phosphate. The organic solvent is dimethyl sulphoxide, N,N-dimethyl formamide, N,N-dimethyl acetamide or N-methyl pyrrolidone.

The invention provides resveratrol based flame retardance epoxy resin. The fully bio-based epoxy resin with flame retardance is prepared by introducing triethyl phosphite and epoxy groups through hydroxyl on resveratrol to form a bio-based epoxy monomer capable of substituting bisphenol A (DGEBA (diglycidyl ether of bisphenol A)) generally used in the industry, synthesizing a higher activity bio-based curing agent, maleopimaric anhydride (MPA), and mixing the curing agent with the prepared epoxy monomer under certain conditions for curing. The epoxy resin is wide in raw material source, greenand environmentally friendly; a synthesis method is relatively simple; the flame retardance of the epoxy resin is good; a maximum limit oxygen index can reach 52%; and a maximum vertical burning gradecan reach V-0. The invention discloses a preparation method of the resin.

A method of preparing for 7-amido-3-ethylene cephalosporanic acid considers 7-phenylacetyl amino-3-chloromethyl cephalosporanic acid p-methoxybenzyl ester (GCLE) as a starting material and adopts the Wittig reaction. Ethylene is introduced on position 3 to obtain 7-phenylacetyl amino-3- ethylene-4- cephalosporanic acid p-methoxybenzyl ester, and a product GVNE is obtained. The GVNE is used to prepare for 7-amido-3-7 alkenyl cephalosporanic acid (7-AVCA). The present invention has the main technical characteristic that the triethyl phosphite with quite low price is used to replace triphenyl-phosphonium in the preparation of the GVNE to realize the purpose of introducing the ethylene on the position 3 of GCLE to prepare for the GVNE. The production method is simple; the cost of the main materials is low; the yield is high; the comprehensive benefit efficiency is high; the present invention is applicable to the large scale industrialized preparation of 7-AVCA.

The invention discloses inflaming retarding polyether polyol, combined polyether, polyurethane foam and a preparation method of the polyether polyol. The preparation method of the polyether polyol includes the steps that first, under the inert atmosphere, diethanol amine, formalin and triethyl phosphite are mixed and reacted, reduced pressure distillation is conducted, and an initiator is obtained; second, the initiator, the polyol, cyanuric acid and a basic catalyst are mixed to obtain feed liquid B; or, the initiator, the polyol, the cyanuric acid and the basic catalyst are mixed to obtain the feed liquid B; or, the initiator, the polyol, the cyanuric acid, the basic catalyst and water are mixed to obtain the feed liquid B; third, the feed liquid B is mixed with epoxide, after the feed liquid B and the epoxide are reacted, feed liquid C is obtained, or dehydration is performed after reacting, and accordingly the feed liquid C is obtained; fourth, the feed liquid C is mixed with epoxide, and the polyether polyol can be obtained after the reaction. The polyether polyol is halogen-free nitrogen and phosphorus collaboration inflaming retarding polyether polyol, the obtained polyurethane foam has good flame retardation, and the preparation method is easy to operate, high in yield and suitable for large-scale industrial production.

A derivative of dibenzo-tetrathiafulvalene-tetrahydroxy-succinimide is provided, which has the structure shown by the right formula, in which R represents an alkyl. The preparation method includes the following procedures that: A) a mixture of dichlorophthalic anhydride and amine with the molecular ratio of 1: 1.5-3 undergoes circumfluence in propionic acid under 140 DEG C to 160 DEG C for 2-4 hours, B) the products obtained in procedure A is mixed with benzyl mercaptan with the molecular ratio of 1:2-3 and then undergoes calefaction in dimethylacetamide under the condition with excessive dosage of K2CO3 under 60 DEG C to 80 DEG C and, C) the product obtained in procedure B is kept in dry toluene with excessive dosage of AlCl3 to undergo debenzylation, and then reacts with carbonyldiimidazole under 70 DEG C to 90 DEG C for 2-5 hours, wherein the molecular ratio between 4,5-[(diphenylmethyl)thio substituted]- phthalimide and the carbonyldiimidazole is 1:1-3 and, D) the product obtained in procedure C undergoes circumfluence in a mixture of toluene/triethyl phosphate, the molecular ratio of which is 2-3/1 to carry out the auto-coupling reaction for 2-5 hours, the product of which is cooled down and filtrated to obtain the target product.

The invention discloses a method for recovering useful constituents such as tetrahydrofuran, methyl diethyl phosphate, triethyl phosphate and trimethylbenzene in a mixed waste solvent during a process of producing glufosinate ammonium by an integrated rectification process. The method comprises the following steps: using an integrated rectification process of discharging and rectifying in a single-tower side line and then connecting a single tower to rectify, directly extracting tetrahydrofuran from the top of the rectification tower in the side line and obtaining trimethylbenzene from the bottom of the tower; extracting the mixed solution of methyl diethyl phosphate and triethyl phosphate from the side line simultaneously, conveying the mixed solution to the rectification tower and carrying out single-tower separation, thereby obtaining methyl diethyl phosphate from the top of the tower and obtaining triethyl phosphate from the bottom of the tower. According to the method disclosed by the invention, the useful constituents in the mixed waste solvent during the glufosinate ammonium production process are recovered by the integrated rectification process, the total recovery rate of the mixed solvent exceeds 98%, and the quality achieves reuse standards. Compared with the conventional three-tower rectification method, the equipment cost and energy consumption of the method disclosed by the invention are obviously lowered.

The invention relates to a reaction type phosphorus-nitrogen flame retardant and in particular to a compound with a plurality of active groups and a preparation method of the compound. The preparation method comprises the following steps: (1) weighing cyanuric chloride, dissolving cyanuric chloride into a first solvent, stirring till being completely dissolved, slowly heating to be 60 DEG C, preserving heat while continuously stirring to uniformly disperse reactant; and (2) in the presence of nitrogen, adding a phosphite ester solution which is dissolved in the first solvent, reacting for 4-6 hours, and keeping stirring in the reaction process. Compared with the prior art, the compound with the plurality of active groups has the beneficial effects that the compound is prepared from raw materials, namely, cyanuric chloride, phosphite ester compounds (trimethyl phosphate or triethyl phosphate) and polyhydric alcohol compounds (neopentyl glycol, glycerol or pentaerythritol) with quaternary carbon (or secondary carbon) atoms, through Michaelis-Arbuzov electrophilic addition reaction and nucleophilic substitution reaction.

A superfine apatite fiber material used for repairing bone tissue is prepared through proportionally mixing triethyl phosphite with distilled water, hydrolyzing while stirring, adding the aqueous solution of calcium nitrate, stirring, ageing to obtain the gel solution, mixing it with alcohol, adding polyvinyl pyrrolidone to obtain the solution for electrospinning, electrospinning, drying and calcining. Its advantages are nano-class fineness, large specific surface area, high biodegradability and high affinity to cells.

The present invention provides a hydrotalcite-tin maleate composite environmental protection stabilizer for PVC, wherein the hydrotalcite-tin maleate composite environmental protection stabilizer is prepared from the following raw materials by weight: 20-30 parts of modified magnesium aluminum hydrotalcite, 10-12 parts of tin maleate, 6-9 parts of lanthanum salicylate, 1-3 parts of triethyl phosphite, 3-6 parts of barium stearate, 2-4 parts of epoxidized soybean oil, 10-13 parts of poly(1,2-propylene glycol adipate), 2-3 parts of beta-diketone, 5-6 parts of isomaltitol, 2-3 parts of 2,4,6-tris(2'n-butoxyphenyl)-1,3,5-triazine, 1-3 parts of oxidized polyethylene wax, and 10-12 parts of celestine powder. According to the present invention, the PVC stabilizer has characteristics of good thermal stability, good processing performance, environmental protection, no toxicity, low cost, good plasticity and balance torque reducing during the PVC processing process, and low cost.

The invention provides a process for preparing triethyl phosphate which comprises, using phsophorus trichloride and absolute alcohol as raw material, synthesizing in benzene solvents, then segregating the expected outcome yield, the synthesis is carried out at the presence of triethylamine. The invention has the advantages of increased yield and improved product purity.

The invention relates to a production method of ethyl-phosphonic acid diethyl ester, which belongs to the technical field of chemical production. Triethyl phosphate is taken as the main material, alkylogen is taken as catalyst, and the ethyl-phosphonic acid diethyl ester is prepared through the processes of charging batch into a reaction kettle, heating up, heat preserving, sampling, cooling and distilling and the like. The equipment for the production of the ethyl-phosphonic acid diethyl ester is simple, and reaction and distillation can be accomplished in a kettle; the product yield is high, no sewage is discharged, and the impact on the environment is small. The method solves the problems that the prior production operating procedure of the ethyl-phosphonic acid diethyl ester is complex, the production cost is high, the environmental pollution is severe and the product yield is low. The invention adopts general chemical equipment, therefore the purchase and maintenance are very convenient. The production cycle is short, and the production of a batch can be accomplished in about 8 hours; the reaction is simple, the triethyl phosphate can be transferred into the final product in one step under the catalysis of the alkylogen, and the transfer efficiency can reach 95 percent.

The invention relates to a preparation method of triethyl phosphate. The method specifically comprises the following steps of: first, with ammonia gas as an acid-binding agent and methyl red as an indicator, reacting phosphorus trichloride with absolute ethyl alcohol to generate triethyl phosphite; filtering out the byproduct ammonium chloride and then, introducing a certain amount of oxygen for oxidization; and finally, distilling and purifying at reduced pressure to obtain the target product triethyl phosphate. The method provided by the invention has the advantages that the yield is high, the unit consumption is low, and the byproduct ammonium chloride can be used as a fertilizer; and the method is simple in production process, the raw materials are easily available and the production safety is high.

The invention discloses a method for catalytically synthesizing dicycloethyl phosphite ester by using ionic liquid, which relates to a method for synthesizing dicycloethyl phosphite ester and solves the problems of long reaction time and low yield during preparing the dicycloethyl phosphite ester by adopting triethylamine as a catalyst. The method comprises the following steps: mixing trimethylolpropane, triethyl phosphite and ionic liquid [Bmim] BF4, then thermostatically reacting the mixture for 1.5 to 5.5 hours under the protection of N2 at the temperature of between 78.4 and 100 DEG C, and distilling the reaction product for 0.5 to 1 hour under reduced pressure to obtain the dicycloethyl phosphite ester. The method for preparing the dicycloethyl phosphite ester has short reaction time, the yield can reach 98 percent, and the purity is 99.27 percent.

The invention discloses a Latamoxef Sodium midbody synthetic method. The method comprises the following steps: a new desulfurizer-triethyl phosphite is adopted for dehydration reaction in toluene and then is subjected to concentrated crystallization to achieve the purpose of synthesizing [1R-[1a, 5a]]-3-methyl-2-(7-oxo-3-phenyl-4-oxa-2, 6-diazabicyclo [3.2.0] heptane-2-alkene-6-based)-3-butenoic acid methyl ester diphenyl. As the triethyl phosphite is selected as the desulfurizer, the technological process is simplified, the operation is simple and the equipment utilization ratio is high.

The invention discloses a 3,5-dimethoxystilbene derivative, a preparation method and an application thereof, in particular relating to the synthesis of the 3,5-dimethoxystilbene derivative as shown in structural formula (1) and anti-drug resistant bacterial activity thereof. The preparation method comprises the following steps: firstly mixing 3,5-dimethoxybenzyl bromide with triethyl phosphate to obtain 3,5-dimethoxybenzyl phosphonate; and then carrying out Wittig-Honner reaction to obtain the 3,5-dimethoxystilbene derivative. The preparation method has the advantages of high yield, simple and convenient operation, low cost, good industrialization prospect and the like. A bacterial inhibiting test result shows that the synthesized 3,5-dimethoxystilbene derivative has obvious inhibition activity on drug resistant bacteria and is of great significance on research and development of a novel anti-drug resistant bacterial drug.

The invention discloses an environment-friendly preparation method of toluylene-based biphenyl type fluorescent brightener, which belongs to the field of a preparation technique of high-grade fluorescent brightener used for washing powder, detergent, cosmetic and the like, and solves the problems of great pollution to the environment and difficulty in disposal in the prior art. The method comprises the steps of: heating and refluxing 4, 4'-bis(chloromethyl)-1, 1'-biphenyl and triethyl phosphite under the condition of N2, distilling to remove a part of triethyl phosphite and side products through vacuum distillation, condensing, and crushing to obtain an esterified product; reacting the esterified product and benzaldehyde-2-sulfonic acid sodium for 2-15 hours in a strong polar aprotic organic solvent and under the action of organic strong base to obtain a condensate; distilling the condensate, recycling the solvent, and recycling tail gases to obtain a condensed mixture; adding water and salt into the condensed mixture, cooling, performing pressure-filtering to obtain a salting-out filter cake, washing, and refining; and drying the refined cake to obtain the toluylene-based biphenyl type fluorescent brightener. According to the method provided by the invention, the recycling is convenient and the brightener can be used circularly; the problem of environmental pollution is solved and energy is saving and the environment is protected; and the used raw materials is convenient in source and low in cost.