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47 results about "Triphosgene" patented technology

Triphosgene (bis(trichloromethyl) carbonate (BTC), C₃Cl₆O₃) is a chemical compound that is used as a safer substitute for phosgene, because, at room temperature, it is a solid crystal, as opposed to phosgene, which is a gas. Triphosgene crystals decompose above 200 °C.

Method and device for continuously synthesizing triphosgene

The invention discloses a triphosgene continuous synthesis method and device, and belongs to the technical field of fine chemical production. The triphosgene continuous synthesis method comprises the following steps: S1, continuously conveying dimethyl carbonate to the lower part of a reactor, and continuously inputting chlorine from the bottom of the reactor; s2, after dimethyl carbonate and chlorine are mixed in a reactor, a reaction is initiated by irradiation of an ultraviolet light source with the wavelength of 295-395 nm, and molten triphosgene and hydrogen chloride gas are generated; wherein the temperature in the reactor is gradually increased from bottom to top to present a temperature gradient; and S3, continuously overflowing the molten-state triphosgene into a degassing tower to remove residual hydrogen chloride in vacuum, and enabling the degassed molten-state triphosgene product to enter a flaking section. According to the method, by optimizing reaction conditions and equipment design, the cost can be reduced, the utilization rate of raw materials can be increased, generation of byproducts can be reduced, meanwhile, the safety and efficiency of the reaction are guaranteed, and efficient, safe and continuous production of triphosgene is achieved.
Owner:SHANDONG GENGCAI NEW MATERIALS TECHNOLOGY CO LTD +1

Preparation method of Linzaagolix

The invention discloses a preparation method of Linzagolix, which comprises the following steps: taking 2, 3-difluoro-6-methoxybenzyl alcohol as a raw material, under the action of alkali and phosphine ligand, carrying out Mitsunobu reaction on 2, 3-difluoro-6-methoxybenzyl alcohol and 2-methoxy-4-fluorophenol to obtain a compound A, sequentially carrying out nitration reaction and reduction reaction on the compound A to obtain a compound C, and carrying out recrystallization on the compound C to obtain the Linzagolix. Under the alkaline condition and the action of triphosgene, the compound C and 4-aminothiophene-2, 3-dimethyl dicarboxylate hydrochloride are subjected to a one-pot condensation reaction to obtain a compound D, and the compound D reacts under the alkaline condition to generate Linzaolix. According to the invention, the synthesis process of Linazagolix is shortened to five steps, the reaction condition is mild, the operation is simpler and more convenient, and the method is suitable for industrial production.
Owner:JINLING PHARMA

Method for synthesizing piperacillin with high selectivity

The invention provides a method for synthesizing piperacillin with high selectivity. The method comprises the following steps: taking ampicillin as an initial raw material, under anhydrous and alkaline conditions, carrying out selective reaction on side chain amino of ampicillin and triphosgene to generate an isocyanate intermediate, and then coupling the intermediate with N-ethyl-2, 3-diketopiperazine to directly obtain piperacillin. The key point of the invention is that the generation of by-products such as self-coupling urea is effectively inhibited by utilizing the characteristics of moderate reaction activity and high selectivity of the isocyanate intermediate. The method has the advantages of simple route, high selectivity, few byproducts, high yield and the like, and provides a more economical and efficient way for industrial production of piperacillin.
Owner:SHANDONG ANSHUN PHARMACEUTICAL CO LTD

Multifunctional compounds based on tris(quinoline-5-methoxy-diachydrazide)benzene, their synthesis and applications

This invention provides a multifunctional compound, TQ5, based on tris(quinoline-5-methoxy-diachydrazide)benzene, for highly sensitive detection of phosgene and triphosgene and efficient separation of heavy metal ions. The concentration is 1×10⁻⁶. ‑5 When triphosgene solution was added to a TQ5 1,4-dioxane solution of M, the fluorescence of the solution at 365 nm changed from colorless to bright green. However, the fluorescence of solutions containing common volatile toxic gases did not change significantly upon addition. The detection limit of triphosgene reached 4.70 × 10⁻⁶. ‑8 M. Similarly, the same mechanism can be used for the detection and identification of highly toxic phosgene. Furthermore, this invention is based on TQ5 compound phosgene fluorescent colorimetric material for convenient, rapid, and highly sensitive detection of triphosgene and phosgene in real-world environments. Finally, TQ5 dry gel powder can be applied to the efficient detection and adsorption separation of heavy metal ions in water, including Cd. 2+ Hg 2+ Ag + The adsorption rates reached 80.85%, 91.64%, and 88.62%, respectively. This study provides a new method for developing multifunctional supramolecular smart materials for multi-substrate detection and separation, which has certain application prospects in the fields of food and environmental safety detection and control.
Owner:NORTHWEST NORMAL UNIVERSITY

High-wear-resistance aliphatic isocyanate and preparation method thereof

The invention relates to high-wear-resistance aliphatic isocyanate and a preparation method thereof, and belongs to the technical field of isocyanate synthesis. 2-methyl-1, 5-pentamethylene diamine is converted into self-made aliphatic isocyanate with steric hindrance through a triphosgene method, sliding of a polyurethane molecular chain is limited, and wear resistance is improved. And compounding with modified nano calcium carbonate treated by a coupling agent to obtain the high-wear-resistance aliphatic isocyanate. And the modified nano calcium carbonate improves the compatibility, avoids agglomeration, enhances interface bonding and further improves the wear resistance. The aliphatic isocyanate prepared by the preparation method disclosed by the invention has a remarkable high wear-resistant effect.
Owner:KUSN ZHONGDI MATERIALS TECH

A preparation method of No. Ⅱ medium fixative

The present invention relates to a preparation method of a No. II neutralizing agent, comprising the following steps: step 1) adding N-methylaniline to an alkaline aqueous solution and mixing to obtain an N-methylaniline mixed solution; step 2) adding bis(trichloromethyl)carbonic acid to the N-methylaniline mixed solution and stirring the reaction; maintaining the reaction temperature less than 105°C by controlling the addition rate of bis(trichloromethyl)carbonic acid during the reaction to obtain a reaction product; step 3) performing solid-liquid separation on the reaction product to obtain No. I neutralizing agent. The present invention uses solid triphosgene as a raw material and adopts a one-pot method to prepare No. II neutralizing agent. The preparation process is stable. When solid phosgene is 105% to 110% of the theoretical feed, the reaction yield can reach more than 95%. At the same time, the entire preparation process is safe, stable, and less polluting during the entire reaction process.
Owner:BEI HUA KAI MING HUAGONG CO LTD

A process for the preparation of a diazabicyclooctene compound

ActiveCN118772145BOrganic chemistry methodsAlkaneAnnulation
The application discloses a preparation method of a diazabicyclooctene compound. Specifically, the method comprises the following steps: performing ring formation reaction of compound 3 and triphosgene in a solvent under the action of a base, as shown in the following formula, and the solvent is a halogenated alkane solvent, and the base is triethylamine. The preparation method has a short synthesis route, reduces consumption of raw materials, and improves overall yield.
Owner:SHANGHAI INST OF PHARMA IND CO LTD +1

Synthesis method of 5-substituted-3, 4-dihydroisoquinoline-1 (2 hydrogen)-ketone

The invention discloses a synthesis method of 5-substituted-3, 4-dihydroisoquinoline-1 (2H)-ketone, which comprises the following steps: a) carrying out condensation reaction on a compound as shown in a formula 2 to obtain a compound as shown in a formula 3; carrying out rearrangement reaction on the compound shown in the formula 3 to obtain a compound shown in a formula 4; and carrying out ring closing on the compound shown in the formula 4 under an acid catalysis condition to obtain a compound shown in a formula 5. The synthesis method provided by the invention avoids the following problems in a known synthesis strategy: raw materials are expensive, and the cost of the whole process is difficult to control; or a highly toxic and easy-to-explode azidation reagent is used, and large-scale production is difficult to realize through an azidation intermediate state with poor stability; therefore, the synthetic method disclosed by the invention is efficient, mild and green, and is more suitable for large-scale production and commercial production.
Owner:HANGZHOU ALLSINO CHEM

Method of producing carbonyl compound and flow type reaction system of producing carbonyl compound

There are provided a method of producing a carbonyl compound by a flow type reaction, including introducing a triphosgene solution into a flow channel (I), bringing the triphosgene solution into contact with a solid catalyst immobilized in at least a part of the flow channel (I) to generate a phosgene solution while the triphosgene solution is flowing through the flow channel (I), joining the phosgene solution and an active hydrogen-containing compound solution that flows inside the flow channel (II), which are subsequently allowed to flow downstream inside a reaction flow channel to be reacted in a presence of a tertiary amine, and obtaining a carbonyl compound in a joining solution; and a flow type reaction system that is suitable for carrying out this production method.
Owner:FUJIFILM CORP

A zinc carbonyl reagent, its preparation method and application

This invention discloses a zinc carbonyl reagent, its preparation method, and its application. The general structural formula of the zinc carbonyl reagent is: where R... 1 R 2 The reagent is independently selected from chain alkyl, cyclic alkyl, substituted alkyl, aryl, or benzyl groups. This invention synthesizes and prepares a zinc carbonyl reagent, which is then applied to the synthesis of urea and thiocarbamate drugs. This provides a new reaction pathway for drug molecule synthesis, and is safe, reliable, and non-toxic. It solves the problem that the synthesis of urea and thiocarbamate drugs in existing technologies requires the use of toxic carbon monoxide, phosgene, and its derivative triphosgene, resulting in a high risk factor in the synthesis process. The synthesis method of this invention uses simple raw materials, has mild reaction conditions, and the synthesized zinc carbonyl reagent can be directly used in the reaction as a solid, making the operation simple.
Owner:SUZHOU UNIV

Formaldehyde fluorescent probe and its preparation method and application

The present invention belongs to the technical field of fluorescent probes, and specifically relates to a formaldehyde fluorescent probe based on formaldehyde-induced catalytic hydrolysis of aminocarboxylic acid hydroxylamine esters, a preparation method thereof, and applications thereof. The preparation of the formaldehyde fluorescent probe specifically comprises the following steps: S1: a naphthalimide derivative A is refluxed with triphosgene and 4-dimethylaminopyridine in a toluene solution to obtain an intermediate B; S2: the intermediate B is reacted with a hydroxylamine derivative C in a dichloromethane solution at room temperature to obtain a probe compound I; the molar ratio of the naphthalimide derivative A, triphosgene, and 4-dimethylaminopyridine in S1 is 1:1.5:3; the molar ratio of the intermediate B to the hydroxylamine derivative C in S2 is 1:1.3; the fluorescent probe of the present invention can selectively and rapidly react with formaldehyde to generate a product with strong fluorescence, and exhibits high selectivity and sensitivity to formaldehyde.
Owner:EAST CHINA UNIV OF SCI & TECH

Preparation method and application of cefepime ester side chain

The application discloses a preparation method of high-purity cephalosporin bipu ester side chain (1a), and a reaction route is shown as follows. The method is characterized in that 2a is used as a starting material to react with triphosgene to generate compound 3a, and then the compound 3a is used to react with p-nitrophenol to generate compound 1a. The product has high purity and high reaction yield, and is suitable for industrial production.
Owner:HUANGGANG LUBAN PHARM

An improved process for the synthesis of oxalyl chloride

This invention relates to the field of organic chemistry, specifically to an improved synthesis process for oxalyl chloride. The provided synthesis process for oxalyl chloride includes the following steps: S1. Adding oxalic acid dihydrate to a reaction vessel and stirring to dissolve; S2. Slowly adding a composite catalyst to the molten liquid from step S1 and stirring until the mixture is homogeneous; S3. Adding triphosgene to the mixture obtained in step S2, while simultaneously introducing nitrogen gas from the bottom of the reaction vessel, and reacting at a temperature between 102 and 108°C for 2-3 hours; S4. Condensing the nitrogen gas overflowing from the reaction vessel in step S3 to obtain crude oxalyl chloride; S5. Releasing the nitrogen gas overflowing from the circulating water condenser after absorption by water and alkali; S6. Purifying the crude oxalyl chloride obtained in step S4 to obtain pure oxalyl chloride. The preparation method of this application is simple, easy to industrialize, and the product yield can reach over 95%, with a product purity of over 99.0%.
Owner:HUBEI BAOSHENGDE PHARM CO LTD

Preparation method of supramolecular nano-imbibition oil displacement agent and application thereof in fracturing

The application discloses a preparation method of a supramolecular nanometer imbibition oil displacement agent and application of the supramolecular nanometer imbibition oil displacement agent in fracturing, and relates to the technical field of oilfield exploitation. Methoxy polyethylene glycol amine is added dropwise into an activated NCA solution prepared by reaction of L-glutamic acid-5-benzyl ester N-carboxylic anhydride and triphosgene, and then is reacted and precipitated to obtain a polyethylene glycol-polybenzyl glutamate block copolymer; the block copolymer is dissolved in a hydrogen bromide solution to obtain a debenzylated product; under initiation of ammonium persulfate, the debenzylated product is reacted with vinyl phosphonic acid to obtain a supramolecular nanometer imbibition oil displacement powder; and the supramolecular nanometer imbibition oil displacement agent is obtained by dissolving, homogenizing and sterilizing filtering the powder. The supramolecular nanometer imbibition oil displacement agent is chelated with calcium and magnesium ions through phosphonic acid groups to form a stable network, so that the supramolecular nanometer imbibition oil displacement agent has long-term and stable effects in high-temperature and high-salt reservoirs; the supramolecular nanometer imbibition oil displacement agent has a flexible size matched with a pore throat structure, and can trigger capillary spontaneous imbibition by using ultralow interfacial tension to achieve efficient oil displacement.
Owner:SHANDONG KEXING CHEM CO LTD

Preparation method and application of scratch-resistant and self-repairing modified polycarbonate

PendingCN120966226APolymer sciencePtru catalyst
The invention belongs to the technical field of modified polycarbonate, and discloses a preparation method of scratch-resistant and self-repairing modified polycarbonate. The method comprises the following steps: uniformly mixing a dichloromethane solution of polysiloxane with an alkali solution of a bio-based monomer in an oxygen-free atmosphere, then adding a dichloromethane solution of triphosgene, and reacting under the action of a first catalyst to prepare a PC-Si prepolymer; adding a dichloromethane solution of a polyurethane prepolymer, a second catalyst and a chain extender into the PC-Si prepolymer to obtain a PU-PC-Si copolymer; and uniformly mixing the PU-PC-Si copolymer, carbon nanotubes, nano-silica, a flame retardant, an anti-UV additive and a slipping agent, and carrying out extrusion granulation to obtain the modified polycarbonate.
Owner:SHENZHEN JIAKAILE IND CO LTD

Continuous production and preparation method of 2-chloro-5-chloromethylpyridine

The invention discloses a continuous production and preparation method of 2-chloro-5-chloromethylpyridine, and belongs to the technical field of synthesis of pesticide intermediates. The method comprises the following steps: continuously introducing 2-chloro-2-chloromethyl-4-cyanobutyraldehyde, a solvent and triphosgene into a two-stage series cyclization reactor, carrying out a reaction at a specific temperature under a negative pressure condition, and timely removing hydrogen chloride generated by the reaction; and after the reaction is finished, extracting the separated tar with a solvent to recover effective components, washing and alkali-washing the obtained organic phase, and desolventizing and distilling the organic phase in a two-stage series film evaporator to obtain the high-purity 2-chloro-5-chloromethylpyridine product. Through full-process continuous operation, the polymerization side reaction is effectively inhibited, the retention time of the material in a severe environment is shortened, the problems of low yield, poor quality and tedious post-treatment in the prior art are solved, the process is efficient and environmentally friendly, the product yield is stabilized to be 90% or above, the product content reaches 96% or above, and the method is suitable for industrial large-scale production.
Owner:ZHONGNONG RUIHUA (GANSU) PHARMACEUTICAL CO LTD +1

Preparation method and application of revienacin key intermediate

The invention discloses a synthesis method and application of a revivacin key intermediate compound shown as a formula I. Reacting 2-aminobiphenyl, triphosgene and N-Boc-4-hydroxypiperidine in an alkaline reagent to obtain a compound as shown in a formula II; the compound shown in the formula II is subjected to deprotection in an acid system to obtain the compound shown in the formula I. The total yield of the two-step reaction is 93-97%, the purity is 99.2-99.8%, and the method does not need a noble metal catalyst, and is mild in reaction condition, low in cost and simple and convenient in post-treatment. And carrying out nucleophilic reaction on the compound shown in the formula I to prepare revienacin.
Owner:CHONGQING SHENGHUAXI PHARMA CO LTD +1

A method for preparing indene diazine compounds and oxadiazine insecticides

PendingCN122325407AIsopropylDiazine
This invention relates to a method for preparing indene diazine compounds and oxadiazine insecticides, belonging to the field of pesticide technology. The structure of the indene diazine compound is shown in Formula II: where R is methyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, phenyl, or a substituted phenyl group. The indene diazine compound shown in Formula II is used to prepare the oxadiazine insecticide shown in Formula I. This invention avoids the use of high-risk materials such as phosgene, triphosgene, and sodium hydride. After multiple batch verifications, the overall reaction yield is stable and suitable for industrial production.
Owner:SHANDONG SHIGAODE PLANT NUTRITION TECH CO LTD

Method for synthesizing Iclepertin

The invention relates to a method for synthesizing Iclepertin, and belongs to the technical field of medicinal chemistry. The reaction route is shown in the specification. Comprising the following steps: (1) carrying out sulfonation reaction on p-fluoroiodobenzene and sodium methanesulfinate to obtain p-fluoromethylsulfonyl benzene; (2) carrying out a reaction on p-fluoromethylsulfonyl benzene and (R)-1, 1, 1-trifluoro-2-propanol to obtain a compound shown in a formula II; (3) reacting the compound shown in the formula IV with triphosgene to obtain a compound shown in a formula III; and (4) carrying out Friedel-Crafts acylation reaction on the compound in the formula II and a compound in a formula III to obtain a compound in a formula I. According to the synthesis method, the reaction route is shortened, high-risk reagents are prevented from being used, and industrial large-scale production is facilitated.
Owner:JINAN NOBOTIN FINE CHEM CO LTD

Triphosgene feeding device

The utility model discloses a triphosgene feeding device which comprises a stirring kettle, a metering pump, a circulating pump, a first connecting pipeline, a second connecting pipeline, a third connecting pipeline and a solid dissolver, wherein triphosgene solids are added into the solid dissolver. The stirring kettle is provided with a gas inlet end, a liquid inlet end and a liquid outlet end, and the liquid outlet end is respectively communicated with the inlet ends of the metering pump and the circulating pump through the first connecting pipeline; the outlet end of the circulating pump is communicated with the inlet end of the solid dissolver through the second connecting pipeline, and the outlet end of the solid dissolver is communicated with the liquid inlet end through the third connecting pipeline; the first connecting pipeline is provided with a feeding inlet control valve used for controlling connection and disconnection of the liquid outlet end and the inlet end of the metering pump. The triphosgene feeding device disclosed by the utility model can ensure that a triphosgene solution is accurately and stably added into a reaction system.
Owner:HEFEI SMOOTHWAY ELECTRONIC MATERIALS CO LTD +2

Olmesartan medoxomil phosgene substitution type acylation reaction system

PendingCN121944951Aavoid safety hazardsprecise automatic controlOrganic chemistrySolution crystallizationOlmesartanReaction temperature
The invention relates to the technical field of drug synthesis equipment, in particular to an olmesartan medoxomil phosgene substitution type acylation reaction system, which comprises a reaction container, a reaction kettle, a reaction kettle and a control system, the triphosgene adding device is connected with the reaction container and is used for quantitatively adding triphosgene into the reaction container; the solvent conveying unit is connected with the reaction container and is used for pumping a solvent into the reaction container; the mixed solution feeding unit is connected with the reaction container and is used for slowly adding a mixed solution of 3-hydroxybutanone and a solvent into the reaction container; the temperature control module is connected with the reaction container and is used for accurately controlling the reaction temperature in the reaction container; and the pH adjusting and quenching unit is connected with the reaction container. According to the invention, the triphosgene adding device and the closed system are adopted to completely replace highly toxic gas phosgene, so that major potential safety hazards in the production, storage and transportation processes are fundamentally solved.
Owner:陕西思伟斯新材料有限公司

Preparation method of drug-linker conjugate

The invention provides a preparation method of a drug-linker conjugate. Specifically, the invention provides a method for preparing a compound IM2, which comprises the following steps: adding a compound SM1 into a mixed solution of triphosgene and 4-dimethylaminopyridine to obtain an intermediate solution; and adding a compound SM2 into the intermediate solution, and stirring to obtain a compound IM2. By optimizing the preparation process of IM2 and using forward chromatography purification which is easy to amplify, the stability, practicability and amplifiability of the process are improved.
Owner:SICHUAN KELUN BIOTECH BIOPHARMACEUTICAL CO LTD

Synthesis method of 6-(methoxy)-3, 4-dihydro-1 (2H)-isoquinolinone

The invention discloses a synthesis method of 6-(methoxy)-3, 4-dihydro-1 (2H)-isoquinolinone, and belongs to the technical field of organic synthesis. The synthesis method comprises the following steps: adding an organic solvent I into a reaction container, then adding triphosgene, controlling the temperature at-10 to 0 DEG C under the protection of inert gas, slowly dropwise adding a solution of dissolving 3-methoxyphenylethylamine into an organic solvent II, keeping the temperature at-10 to 0 DEG C, adding alkali, keeping the temperature and stirring, then adding trifluoromethanesulfonic acid, cooling to-30 to-10 DEG C, stirring and reacting, cooling to-30 to-10 DEG C, cooling to-30 to-10 DEG C, filtering, washing, and drying to obtain the 3-methoxyphenylethylamine. And carrying out post-treatment on the obtained reaction liquid to obtain the product. According to the method, the 6-(methoxy)-3, 4-dihydro-1 (2H)-isoquinolinone is generated through a one-pot method at a high conversion rate, the synthesis cost is low, the steps are simple and short, the reaction conditions are mild, the method is suitable for industrialization, and a potential route is provided for large-scale production of the 6-(methoxy)-3, 4-dihydro-1 (2H)-isoquinolinone.
Owner:KEMEC (SHANGHAI) PHARM TECH CO LTD

Preparation of COF-polyamide hybrid nanofiltration membrane and application of COF-polyamide hybrid nanofiltration membrane in wastewater treatment

The invention discloses preparation of a COF-polyamide hybrid nanofiltration membrane and application of the COF-polyamide hybrid nanofiltration membrane in wastewater treatment, and belongs to the technical field of water treatment separation membranes. The preparation method of the COF-polyamide hybrid nanofiltration membrane comprises the following steps: 1) synthesizing a COF layer on a polyacrylonitrile (PAN) substrate through an in-situ growth method; and 2) introducing trimesoyl chloride (TMC) and piperazine (PIP) on the COF / PAN substrate, and synthesizing the COF-polyamide hybrid nanofiltration membrane on the surface of the COF layer through an interfacial polymerization process (IP). The COF-polyamide hybrid nanofiltration membrane prepared by the invention contains an electronegative functional group carboxyl, and the density of negative charges on the surface of the membrane is improved by protonation of the COF-polyamide hybrid nanofiltration membrane, so that the Doonan effect of the nanofiltration membrane is enhanced, and efficient interception of divalent anions is realized. In addition, the synthesis method is simple to operate, simple in process, low in cost and suitable for large-scale preparation and use, and has good practical value.
Owner:NORTH CHINA ELECTRIC POWER UNIV

A new process for the continuous production of carbamazepine

The application discloses a new process for continuously preparing carbamazepine, and comprises the following steps: (1) dissolving indole in an organic solvent as raw material liquid I, filling a copper catalyst and the like in a tubular reactor, and reacting the raw material liquid I through the tubular reactor to obtain a reaction liquid, and distilling the reaction liquid to obtain 1-phenylindole; (2) dissolving 1-phenylindole and an acid catalyst in organic solvents respectively as raw material liquids II and III, mixing and reacting the raw material liquids II and III through a tubular reactor to obtain a reaction liquid, and recrystallizing the reaction liquid to obtain imino stilbene; (3) dissolving imino stilbene and triphosgene in organic solvents as raw material liquids IV and V, mixing and reacting the raw material liquids IV and V through a tubular reactor, mixing and reacting the reaction liquid with ammonia water again, and finally recrystallizing the reaction liquid to obtain carbamazepine; the process has three steps of reaction in total, the yield of each step is above 85%, the reaction speed is fast, the side reaction is less, the mass transfer and heat transfer efficiency is high, the safety is high, the waste is less, the cost is low, and the post-treatment is convenient.
Owner:ZHEJIANG UNIV OF TECH

Triphosgene solid feeding device in lopinavir intermediate TPA production process

The utility model discloses a triphosgene solid feeding device in the production process of lopinavir intermediate TPA, and belongs to the technical field of feeding devices, the triphosgene solid feeding device comprises a feeding unit and an adjusting unit, the adjusting unit comprises a material guide cylinder, a table-shaped feeding cylinder is fixedly mounted at the top of the material guide cylinder, and a feeding port is formed in the top of the table-shaped feeding cylinder. The adjusting unit comprises a sealing groove formed in the inner wall of the material guiding barrel, an adjusting plate is fixedly installed on the outer wall of the material guiding barrel and is parallel to the sealing groove, the side face of the adjusting plate is open and penetrates through the material guiding barrel, and a circular sealing plate is slidably installed in the adjusting plate; the adjusting plate is fixedly installed on the inner wall of the sealing plate, a reset spring is fixedly installed on the inner wall of the adjusting plate, the other end of the reset spring is fixedly connected with the inner wall of the sealing plate, an inserting groove penetrating through the adjusting plate is formed in the end, away from the sealing plate, of the adjusting plate, and a positioning groove is formed in the outer wall of the inserting groove. And the channel is changed along with the change of the material state.
Owner:XIAMEN SICHONG BIOPHARMACEUTICAL TECHNOLOGY CO LTD

Method and system for continuously synthesizing triphosgene by taking silicon tetrachloride as solvent

The invention discloses a method and a system for continuously synthesizing triphosgene by taking silicon tetrachloride as a solvent, and belongs to the technical field of fine chemical production. The triphosgene continuous synthesis method comprises the following steps: S1, mixing dimethyl carbonate and liquid silicon tetrachloride according to a preset proportion, and continuously conveying the mixture to the lower part of a reactor; s2, chlorine is introduced from the bottom of the reactor according to a preset proportion; s3, initiating a chlorination reaction in the reactor through irradiation of an ultraviolet light source; s4, conveying a mixed solution of the reaction product triphosgene and silicon tetrachloride to a normal-pressure flash tank, gasifying and separating the silicon tetrachloride, condensing and recovering the silicon tetrachloride to a solvent recovery tank, and outputting a molten triphosgene product. Silicon tetrachloride is used as a reaction solvent, so that on one hand, the effects of dispersing and diluting materials and reducing the reaction intensity can be achieved, on the other hand, silicon tetrachloride can be used as a heat removal agent, reaction heat is removed out of a reaction system in a mode of absorbing the reaction heat to gasify the silicon tetrachloride, and the safety and controllability of the continuous synthesis reaction process of triphosgene are achieved.
Owner:SHANDONG GENGCAI NEW MATERIALS TECHNOLOGY CO LTD +1

A continuous method and apparatus for the synthesis of triphosgene

A continuous synthesis method and device of triphosgene belong to the technical field of fine chemical production. The continuous synthesis method of triphosgene comprises the following steps: S1, continuously conveying dimethyl carbonate to the lower part of a reactor, and continuously inputting chlorine from the bottom of the reactor; S2, after the dimethyl carbonate and the chlorine are mixed in the reactor, a reaction is initiated by irradiation of an ultraviolet light source with a wavelength of 295-395 nm, to generate molten triphosgene and hydrogen chloride gas; wherein the temperature in the reactor gradually increases from bottom to top, presenting a temperature gradient; S3, the molten triphosgene continuously overflows to a degassing tower to remove residual hydrogen chloride under vacuum, and the molten triphosgene product after degassing enters a flaking section. Through optimization of reaction conditions and equipment design, the application can reduce cost, improve the utilization rate of raw materials, reduce the generation of by-products, while ensuring the safety and efficiency of the reaction, and realize efficient, safe and continuous production of triphosgene.
Owner:SHANDONG GENGCAI NEW MATERIALS TECHNOLOGY CO LTD +1

Preparation method of D-dihydrophenylglycine methyl ester hydrochloride

The invention provides a preparation method of D-dihydrophenylglycine methyl ester hydrochloride, and belongs to the technical field of pharmaceutical chemicals. Deoxidizing the reactor, adding methanol and D-dihydrophenylglycine, and stirring and dispersing; adding triphosgene in batches under the conditions of nitrogen protection and-5 to 10 DEG C, and heating to 50 to 60 DEG C to carry out esterification reaction after the triphosgene is completely added; when it is detected that the conversion rate of D-dihydrophenylglycine reaches 96% or above, the esterification reaction is finished, and methanol is subjected to reduced pressure distillation until a dry solid is obtained; controlling the decompression temperature to be below 60 DEG C, adding a solvent sleeve to distill residual methanol, adding the solvent again to disperse and cool the solid, and cooling; and filtering and drying in vacuum to obtain the finished product D-dihydrophenylglycine methyl ester hydrochloride. The one-time yield of the method is greater than 90%, and the method can be used for the cefradine enzymatic side chain and has a great industrialization prospect.
Owner:ZHEJIANG ANGLIKANG JINHE BIOTECHNOLOGY CO LTD +1

A synthetic method for cyantraniliprole impurity

The invention discloses a method for synthesizing a cyantraniliprole impurity. The chemical name of the impurity is 3-bromo-1-(3-chloro-2-pyridyl)-N-[4-(formamido)-2-methyl-6-[(methylamino)carbonyl]phenyl]-1-hydrogen-pyrazole-5-carboxamide. 2-amino-3-methylbenzoic acid is used as a starting material, and the product is sequentially subjected to triphosgene cyclization, nitration, amine transesterification ring-opening, hydrogenation reduction, and two-step amide condensation reactions to finally obtain a target compound, 3-bromo-1-(3-chloro-2-pyridyl)-N-[4-(formamido)-2-methyl-6-[(methylamino)carbonyl]phenyl]-1-hydrogen-pyrazole-5-carboxamide. The whole reaction route has simple conditions, is easy to operate, and is economical and practical.
Owner:JIANGSU AIKEMU TESTING CO LTD