26 results about "Triphosgene" patented technology

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.

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.

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.

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.

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.

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.

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%.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

The preparation method of the ether isocyanate and polyurethane associated thickener comprises the following steps: S1, adding a dihydric alcohol compound and an organic strong base, and heating to 60 DEG C; dropwise adding acrylonitrile, and stirring until the reaction is complete; s2, transferring the product in S1 into a high-pressure kettle, adding Raney nickel and methanol, and reacting to obtain ether diamine; and S3, dissolving ether diamine and triethylamine in dry dichloromethane, dropwise adding a dichloromethane solution containing triphosgene, and reacting to obtain the ether isocyanate. S4, adding polyethylene glycol, replacing gas, heating to 100 DEG C, and dehydrating polyethylene glycol until the water content is less than 0.01 wt%; and S5, adding an auxiliary agent and ether isocyanate, and adding monohydric alcohol for end-capping reaction. According to the invention, a class of ether isocyanate with a novel structure is synthesized, the polyurethane associated thickener based on the isocyanate is prepared from the ether isocyanate, the hydrophilic segment property of the associated thickener is more excellent than that of common isocyanate, and the performance of the final thickener is more adjustable and controllable.

The invention relates to the technical field of 4, 6-dichloro-2-phenylpyrimidine synthesis, in particular to a 4, 6-dichloro-2-phenylpyrimidine green synthesis process based on triphosgene substitution, which comprises the following steps: step 1, raw material selection and pretreatment work; step 2, dissolving raw materials and adding a catalyst; 3, carrying out a chlorination reaction and introducing phosgene; step 4, post-treatment and purification treatment; step 5, recycling and purifying by-products; according to the invention, the triphosgene is adopted to replace highly toxic and easily-leaked gaseous phosgene and highly-corrosive phosphorus oxychloride as a chlorinating agent, and the triphosgene is stable at normal temperature, so that the safety risk in the production, storage and operation processes is greatly reduced, and the dependence on special equipment and harsh safety management is avoided; the process is easier and safer to realize industrial large-scale production; a high-quality product with the purity being greater than or equal to 99.8% is obtained through systematic purification; a complete resource circulation system is established, and green production is realized.

The application discloses a furan oxadiazole ketone compound and a preparation method and application thereof in detecting CO3 2‑ or PO4 3‑ . The furan oxadiazole ketone compound has a structural formula. The application further provides a preparation method of the furan oxadiazole ketone compound, which comprises the following steps: reacting 5-nitrofuran-2-carboxylic acid and oxalyl chloride to obtain 5-nitrofuran-2-carbonyl chloride, then acylating 2-hydrazinyl pyrimidine with 5-nitrofuran-2-carbonyl chloride to obtain 5-nitro-N'-(2-pyrimidinyl) furan-2-carbonyl hydrazine, and forming a ring of the 5-nitro-N'-(2-pyrimidinyl) furan-2-carbonyl hydrazine with triphosgene to obtain the furan oxadiazole ketone compound. The furan oxadiazole ketone compound provided by the application is an optical probe, which can be used as a fluorescent probe to detect CO3 2‑ or PO4 3‑ in environmental water bodies, and has strong anti-interference ability.

The invention provides an adamantane carbonate derived photoacid generator and a preparation method thereof.The method comprises the steps that triphosgene serves as a substrate, the triphosgene, adamantane methanol and organic alkali are dissolved in an organic solvent, after substitution reaction is conducted under the temperature control condition, reaction liquid is filtered and subjected to reduced pressure distillation, and a chloroformate adamantane methyl ester intermediate is obtained; the preparation method comprises the following steps: reacting an intermediate with 2-fluoro-2-bromoethanol and organic alkali in dichloromethane at a controlled temperature to obtain 1-adamantane methyl carbonate 2-bromo-2-fluoroethyl ester oily matter, sulfonating the oily matter to obtain a 1-adamantane methyl carbonate 2-fluoroethyl ester sodium sulfonate carbonate compound, and reacting the compound with 4-[1-(4-methoxybenzoyl)-2, 2, 4-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3 The preparation method comprises the following steps: carrying out anion exchange reaction on 2, 2-dimethylpropyl]-[1, 4] oxathietidine-4-onium trifluoroacetate in a mixed system of dichloromethane and water, concentrating an organic phase, and finally crystallizing isopropyl ether to obtain a target product.

The invention discloses a method for continuously preparing 9-fluorenylmethoxycarbonyl succinimide, which comprises the following steps: S1, (1) dissolving 9-fluorenylmethanol and an organic alkali reagent in an organic solvent A to form a solution A; (2) dissolving triphosgene in an organic solvent B to form a solution B; (3) dissolving N-hydroxysuccinimide and an organic alkali reagent in an organic solvent C to form a solution C; s2, mixing the solution A and the solution B at a first constant flow rate, and enabling the mixture to enter a first microchannel continuous flow reactor for chloroformylation reaction to obtain a reaction intermediate Fmoc-Cl; s3, mixing the solution C with the reaction intermediate Fmoc-Cl at a second constant flow rate, and enabling the mixture to enter a second microchannel continuous flow reactor for esterification reaction to prepare 9-fluorenylmethoxycarbonyl succinimide; and S4, after the reaction, concentrating the reaction effluent to remove the organic solvent, extracting, recrystallizing, filtering and collecting white crystals, and drying in vacuum to obtain the product 9-fluorenylmethoxycarbonyl succinimide.

The invention discloses a preparation method of a 1, 5-dihydro-2, 4-benzodiazepine-3-ketone derivative, raw materials required by the preparation method are cheap and easy to obtain, the use of an inflammable and explosive reagent borane, a highly toxic reagent triphosgene which is not easy to operate and precious metal palladium is avoided, meanwhile, the operation is simple and convenient, the production cost is reduced, and the preparation method is more suitable for industrial preparation and use. The yield is higher than that in the prior art. Meanwhile, the invention also discloses an intermediate as shown in the formula III for preparing the derivative or a salt thereof and a preparation method thereof.

The application discloses a kind of COF-polyamide hybrid nanofiltration membrane preparation and wastewater treatment application, belong to water treatment separation membrane technical field.The preparation method of the COF-polyamide hybrid nanofiltration membrane includes:1) by in-situ growth method on polyacrylonitrile (PAN) substrate synthesis a layer of COF layer;2) on COF / PAN substrate, introduce triphosgene (TMC) and piperazine (PIP) in COF layer surface by interfacial polymerization process (IP) synthesis COF-polyamide hybrid nanofiltration membrane.The COF-polyamide hybrid nanofiltration membrane prepared in the application contains negative electric functional group carboxyl, and the density of membrane surface negative charge is improved by protonation, to enhance the sonne effect of nanofiltration membrane, realizes the efficient interception to divalent anion.In addition, this synthesis method is simple in operation, process is simple, low in cost, suitable for large-scale preparation use, with good practical value.