453 results about "Triphosgene" patented technology

The invention discloses a method for preparing avibactam sodium through a one-pot method. The method comprises the following steps: by taking (2S,5R)-5-[(benzyloxy)amino]pyridine-2-ethyl carboxylate oxalate as a starting material, firstly generating a compound II by reacting with triphosgene, hydrolyzing, adding ammonia water to perform ammoniation, thereby obtaining a compound III, performing hydrogenation by taking formic acid, ammonium formate or hydrazine hydrate as a hydrogen donor in hydrogenation reaction, and then salifying to obtain the avibactam sodium. The avibactam sodium is prepared by use of the one-pot method, the raw material is cheap and easy to obtain, the reaction condition is mild, the operation is simple, the safety is higher, the yield is high, the purity is good, and the method is suitable for large scale industrial production. Formulae are shown in the description.

The invention discloses a sucralose green synthesizing method, which uses cane sugar as raw materials, adds ionic liquid for esterification reaction with acetic anhydride under the action of acid catalyst to generate cane sugar-6-acetic ester, which is chloro-substituted by solid triphosgene and degreased in ionic liquid to generate the sucralose. The invention has the advantages that the process is environment-friendly, the product quality is excellent, the operation is simple and the production cost is low, which is an ideal process for industrialized production.

The invention relates to a method for synthesizing a beta-lactamase inhibitor Avibactam and belongs to the technical field of preparation of beta-lactamase inhibitors. The method disclosed by the invention comprises the following steps: (1) taking a compound 2 as a raw material, and reacting with R<1>NH2 so as to produce a compound 3; (2) enabling the compound 3 and a biocatalyst to produce a compound 4 in an organic solvent in the presence of glucose or sucrose; (3) enabling the compound 4 to react with trifluoroacetic anhydride so as to obtain a compound 5; (4) enabling the compound 5 to react with R<2>ONH2 so as to produce a compound 6; (5) hydrolyzing the compound 6 under alkaline conditions so as to produce a compound 7; (6) enabling the compound 7 to react with triphosgene so as to produce a compound 8; (7) enabling the compound 8 to react with ammonium formate in the presence of a catalyst so as to produce a compound 9 in the organic solvent, wherein the catalyst is a Pd/C system; and (8) enabling the compound 9 to react with a sulfonating agent, thereby obtaining the product 1. The method disclosed by the invention is stable in process, high in yield, simple and safe in operation and low in production cost.

The invention relates to a method for preparing rivastigmine hydrogen and tartrate thereof, which comprises the following steps: taking metamethoxyacetophenone as an initial raw material, and obtaining 1-(3-methoxyphenyl)ethanol by the reduction; then performing the chlorination to obtain 1-(chloroethyl)-3-methoxyphenyl; then reacting the1-(chloroethyl)-3-methoxyphenyl with dimethylamine hydrochloride to obtain 1-(3-methoxyphenyl)-N, N-dimethylethanamine; demethylating the reaction product to obtain 3-[1-(dimethylamino)ethyl]phenol; then performing salt formation resolution with (s)-(+)-camphor-10-sulfonic acid, recrystallizing, and dissociating to obtain (s)-3-[1-(dimethylamino)ethyl]phenol; then taking ethylamine as a raw material to react with ethyl formate to obtain formylethylamine; then reacting the formylethylamine with phosphorus oxychloride to obtain an imine intermediate; reducing the imine intermediate by sodium borohydride to obtain ethyl methyl amine; then reacting the ethyl methyl amine with triphosgene to obtain N-methyl-N-ethylformyl chloride; and finally using (s)-3-[1-dimethylamino)ethyl]phenol to condensate with the N-methyl-N-ethylformyl chloride, and then performing salt formation with levotartaric acid to obtain the rivastigmine hydrogen tartrate. The method has the advantages of easily-obtained raw materials, simple and convenient operation, low cost, high yield and small pollution, and is a brandnew synthesis route at present.

The present invention relates to synthesis of dipeptide containing amino acid, and provides a kind of synthesis process of N(2)-L-alanyl-L-glutamine dipeptide with low material cost, simplicity, high yield, no need of separating and purifying intermediate product, easy product separation and purification and environment friendship. The synthesis process includes the reaction of amino acid with protected N-terminal with phosphorus triphenyl oxide and triphosgene in organic solvent to form active ester; the reaction of the active ester with glutamine in water solution of inorganic alkali; acidifying with inorganic acid and eliminating N-terminal protecting radical.

The invention provides synthesis of amphipathic block antibacterial peptide as well as a preparation method and application of an assembly of the amphipathic block antibacterial peptide. The amphipathic block antibacterial peptide is prepared from hydrophilic amino acid, hydrophobic amino acid, triphosgene, an organic solvent, an initiator, a de-protection agent and a precipitant. The amphipathic block antibacterial peptide provided by the invention has broad-spectrum and excellent antibacterial properties, is an economic, low-toxic and stable biological material, has wide application prospects and values, is low in raw material price, easy in raw material obtaining and low in cost, and in addition, the synthesis is simple in route and controllable in condition.

The invention discloses a method for synthesizing 3,5-dichlorobenzoyl chloride. The method comprises the following steps: carrying out sulfonation on benzoyl chloride by sulfur trioxide to obtain 5-chloroformyl metaphenylene disulfonic acid; carrying out chlorination by catalyzed triphosgene to obtain 5-chloroformyl metaphenylene disulfuryl chloride; finally, carrying out removal of sulfur dioxide chlorination to obtain 3,5-dichlorobenzoyl chloride. Compared with an existing preparation method, the method disclosed by the invention has the characteristics of stable chlorinating agent, high production safety, small amount of three wastes, no requirement for recovering and treating a great amount of dangerous byproducts, no requirement for refining a coarse product, low production cost and the like and is suitable for industrial production.

In one embodiment of the invention a method to prepare sucralose-6-acylate through chlorinating sucrose-6-acylater by BTC in the process of sucralose preparation is disclosed. In this embodiment a Vilsmeier reagent is firstly prepared below 0° C. by dissolving BTC in DMF or in component solvent, containing DMF, toluene, dichloroethane, chloroform and carbon tetrachloride. Consequently, sucrose-6-ester was chlorinated by Vilsmeier reagent. BTC can also be dissolved in one or several organic solvent such as toluene, dichloroethane, chloroform and carbon tetrachloride, and added to a DMF solution of sucrose-6-acylate for chlorination. Sucralose was prepared through de-esterifying the obtained sucralosed 6-ester using sodium methoxide/methanol or sodium ethoxide/ethanol.

The invention discloses a phenyl piperazidine heterocyclic medicinal compound. The compound has high affinity to a dopamine D3 receptor, so that the compound can be used for treating addiction to and dependence on medicines such as cocaine, and a central nervous system disorder relevant to the addiction and the dependence. The compound is a 4-[4-(substituted phenyl) piperazine piperazinyl-1]-butylcarbamic acid substituted aromatic ester derivative with a structural formula as Formula (1) as shown in the specification. A synthetic method of the derivate comprises the steps that substituted aniline and 2-(beta-chloroethyl) amine hydrochloride reacts in a solvent by taking inorganic base as an acid-binding agent to form corresponding substituted phenyl piperazidine hydrochloride 1; substituted phenyl piperazidine hydrochloride 1 and N-(delta-bromobutyl) phthalimide react in acetonitrile by taking K2CO3 as an acid-binding agent and under catalysis of KI to form a reaction intermediate 2; the intermediate 2 is subjected to hydrazinolysis to form an intermediate 3; and the intermediate 3 and an intermediate 5 are condensed by taking triethylamine as an acid-binding agent and a catalyst to form a target product I. The intermediate 5 is obtained in a manner that triphosgene and substituted aromatic phenol conduct partial condensation reaction in methylene chloride.

A process for synthesizing phosphine triphenyldichloride features the reaction between phosphine triphenyloxide and triphosgene or biphosgene in organic solvent under existance of the nucleophilic catalyst chosen from N,N-dimethyl formamide, triethylamine, pyridine, etc.

The invention relates to a pyridylurea biquaternary ammonium salt as well as a preparation method and application thereof. The preparation method of the pyridylurea biquaternary ammonium salt comprises the following steps: using 3-aminopyridine as a staring material, conducting reaction on 3-aminopyridine and triphosgene to obtain 1,3-bi(3-pyridyl)urea, and conducting reaction on 1,3-bi(3-pyridyl)urea and alkyl bromide under the solvent-free condition to prepare the pyridylurea biquaternary ammonium salt. According to the method, a solvent-free method is adopted to prepare the pyridylurea biquaternary ammonium salt, so that the environment can be protected, and the yield is relatively high. The provided pyridylurea biquaternary ammonium salt can be used as a plant growth regulator to promote plant cell division, and the problem that the traditional phenylurea plant growth regulator is poor in water solubility is solved.

The invention discloses a method for preparing paratoluensulfonyl chloride, which comprises the following step of: reacting paratoluenesulfonic acid ammonium salt with bis(trichloromethyl) carbonate (commonly called triphosgene) in an inert organic solvent under the condition that organic alkali is used as a catalyst to synthesize the paratoluensulfonyl chloride. The preparation method has the advantages that: raw materials are conveniently and readily available, the process is simple and suitable for scale-up production, reaction conditions are mild, and a product is easy to purify. The prepared paratoluensulfonyl chloride is an important fine chemical product and can be used for preparing a dye intermediate, synthesizing intermediates of more than ten kinds of antibacterial medicines and anti-inflammatory medicines such as betamethasone, sulfamylon and the like and synthesizing plastic plasticizers, resin, coatings, pesticides and light-sensitive materials.

The invention relates to a new method for preparing a cefuroxime sodium compound. A target product is prepared by using triphosgene and triphenylphosphine oxide as catalysts, reacting 7-amino-cephalosporanic acid with (Z)-methoxyl imido furylacetic acid ammonium salt and sequentially adding chlorosulfonyl isocyanate and sodium iso-octoate for reaction. The cefuroxime sodium compound prepared by the method is greatly enhanced in purity and yield coefficient and has advantages of inexpensive using materials, simple synthesizing technology and equipment and easy production separation and purification.

The invention relates to a preparation method for phthalyl chloride, m-phthaloyl chloride and paraphthaloyl chloride. In the method, benzene dicarboxylic acid and triphosgene are taken as raw materials and mixed for catalytic reaction in an organic solvent of 1, 2-dichloroethane, the mol ratio for the catalytic reaction is 0.5-0.9, the catalyst is N, the dosage of N-dimethyl formamide is 0.1-0.6 time of the weight of the raw material benzene dicarboxylic acid, the catalytic reaction lasts for 2-5 hours, and the reaction temperature is the reflux temperature of the solvent 1, 2-dichloroethane. Compared with the prior art, the invention avoids using toxic and hazardous thionyl chloride, phosphorus oxychloride and phosgene and the like. Therefore, the invention has the advantages of reasonable process conditions, simple and safe operation, high reaction yield, low manufacture cost and easy realization of industrial production, and has high implementation value, social benefit, economic benefit and environmental benefit.

The invention provides a method for synthesizing chlorinated formic acid 9-fluoren methyl, which comprises the following steps: (1) 9-fluoren methyl and triphosgene are reacted for 0.5 to 3 hours in ice bath, under the existence of catalyst and in organic solvent; the catalyst is chosen from N with nucleophilicity, N-dimethylformamide, acetone, diisopropyl ethyl amine, diethylamine, triethylamine, ethyleendiamine, putrescine, imidazole, and the solvent is chosen from benzene, toluene, cyclohexane, hexane, heptane, cyclopentane, dichloromethane, chloroform and the compound thereof; (2) the temperature raises to 20 to 50 DEG C, and the mixture reacts for 1 to 5 hours. The method for synthesizing chlorinated formic acid 9-fluoren methyl adopts safe solid phosgene as reactant, and is simple in technique, convenient in safety, mild in condition, high in yield and easy in realization of industrialization production; the solvent can be used repeatedly after being processed simply, and the products do not need to be refined, and purity is up to more than 98 percent.

This invention discloses a synthetic method of extra high molecular weight polycarbonate. Materials are three phosgene and bisphenol A, it includes condensation polymerization, washing, sedimentation and separating each unit processes. The condensation polymerization is that soduim salt water solution of bisphenol an or its soduim salt solid is proceeded liquid-liquid two-phase polycondensation or solid-liquid two-phase suspension polycondensation 3-5 hours under temperature 20-450C with dichloromethane solution of three phosgene with phase transfer catalyst and tertiary amine and spreading agent. The mole ratio of bisphenol an and three phosgene is 1:0.3-0.5. Viscosity-average molecular weight of polycarbonate >70,000, yield that count by bisphenol A >= 98% and by three phosgene >= 85%. The reaction is milden, smooth and is reacted at normal temperature and normal pressure, and operation and control is simple, security is high, and it is appropriate to industrial production.

The invention relates to a preparation method of 2-chloro-5-picoline. According to the method, benzyl chloride is taken as a raw material, benzaldehyde is taken as an inhibitor, ammonia is taken as an aminating agent, a product has a condensation reaction with propionaldehyde under the catalysis of an organic base, then a product has acetylation with an acetylation reagent, finally, a product performs cyclization under actions of N,N-dimethylformamide and triphosgene, and the target product 2-chloro-5-picoline is obtained through purification. The product purity is higher than or equal to 99.5%, and the total molar yield higher than 80% is realized. The preparation method of 2-chloro-5-picoline has good reaction selectivity, high yield and few three wastes, is simple to operate and facilitates industrialized production.

Production of diphenyl carbonate from trichloromethyl-carbonate ester adopts tubular reactor to increase contact effect and has more yield.

The invention relates to the technical field of heterocyclic chemistry, especially relates to a condensed ring system containing oxygen atoms as the only heterocycle atoms, concretely discloses a preparation method of a Darunavir intermediate. The method comprises the following steps: obtaining a compound of formula (3) by using (3R,3aS,6aR)-hexahydro-furo[2,3-b]furan-3-ol as a raw material to react with triphosgene under alkaline conditions, then directly reacting with a compound of formula (7) to obtain a compound of formula (8); or obtaining a compound of formula (3) to react with an N-hydroxyl compound to prepare active ester, and then reacting with the compound of formula (7) to obtain the compound of formula (8).

The invention relates to a fluorescent probe and in particular relates to a fluorescent probe for detecting nitrogen monoxide and a preparation method thereof. The probe uses 4-amino-1,8-naphthalimide as a basic molecular structure and carbamided o-phenylenediamine as a compound with nitrogen monoxide recognition groups. The preparation method comprises the following steps: adding 4-amino-1,8-naphthoic anhydride and an organic solvent into a container, then adding 2-(2-aminoethoxyl)ethanol, heating for reaction, and cooling; adding a saline solution, centrifuging to obtain an intermediate A, then dissolving the intermediate A in pyridine, and adding acetic anhydride to react; performing rotary evaporation, and adding water for extraction; performing rotary evaporation to separate out an intermediate B; adding the intermediate B, diisopropylethylamine and toluene into a container to obtain a mixed solution, then adding the mixed solution in a solution containing triphosgene and toluene, heating for refluxing, and cooling; adding dichloromethane, carrying out centrifugal separation to obtain a supernatant, and then adding the supernatant into a solution containing o-phenylenediamine and dichloromethane to react; performing rotary evaporation, and adding water for extraction; and drying the obtained ethyl acetate, and performing rotary evaporation to separate out the product.

The invention discloses a preparation method of trialkoxy siloyl isocyanate, comprising the following steps: (1) chlorine catching agent is dissolved in water and then is added into a reaction device to be stirred, wherein, the temperature is controlled at -5-0 DEG C; (2) triphosgene and trialkoxysilane amine are respectively dissolved in organic solvent and then respectively added into the reaction device and react by stirring for 10-20min, wherein, the temperature is controlled at -5-10 DEG C; (3) the phase separation is carried out on the reacted solution, the organic solvent is used for extracting water phase for 1-3 times, the drying is carried out after organic phases are annexed, and the organic solvent is extracted, filtered and removed; (4) after the vacuum distillation, the trialkoxy siloyl isocyanate is obtained. The chlorine catching agent used by the invention has the advantages of cheap price and low production cost. The used triphosgene has the advantages of no toxicity, safety and reliability.

The invention relates to a preparation method of ponazuril which is an anti-coccidiosis drug. The method includes syntheses of 3-methyl-4-(4-phenoxy trifluoromethyl sulfide)-nitrobenzene, 3-methyl-4-(4-phenoxy trifluoromethyl sulfide)-aniline, 3-methyl-4-(4-phenoxy trifluoromethyl sulfide)-phenyl isocyanate, 1-[3-methyl-4-(4-phenoxy trifluoromethyl sulfide)-m-methylphenyl]-1,3,5-triazine-2,4,6-trione and ponazuril. Dangerous articles such as raney nickel, methyl isocyanate, chloroformylisocyanate, phosgene, triphosgene and hydrazine hydrate are not used during the reaction processes, and the operation is safe and reliable; raw materials are easy to obtain, the production cost and pollution are low, and the production process is environment-friendly; and the preparation method is simple, special equipment is not needed, a total yield of ponazuril product can reach above 60%, and large-scaleindustrial production is facilitated.