65 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 present invention relates to a method for preparing 4,4'-difluorobenzophenone from 4-chlorofluorobenzene, which comprises the following steps: (1) Using 4-chlorofluorobenzene as the starting material, reacting with magnesium chips in a solvent to prepare a 4-fluorophenylmagnesium chloride solution; (2) Adding the 4-fluorophenylmagnesium chloride solution to a triphosgene solution, and reacting to obtain the target product 4,4'-difluorobenzophenone. In the present invention, the ketone carbonyl group is introduced through triphosgene, the reaction conditions are mild, the Friedel-Crafts reaction or diazotization reaction can be avoided, the use of aluminum trichloride or the generation of diazonium salts with explosion hazards can be avoided, the environmental pollution is small, the operation is safe and simple, and there is no corrosion to the equipment; the starting material 4-chlorofluorobenzene used has a wide source and low cost; the present invention has high yield and repeatability and is easy to be industrially produced.

The preparation method comprises the following steps: 1, adding tartaric acid, an acid-binding agent and a first organic solvent into a reaction container, uniformly mixing, cooling, dropwise adding a mixed solution of triphosgene and the first solvent into the reaction container under the condition that the temperature does not exceed 10 DEG C, and reacting for 1-2 hours at the temperature of 20-30 DEG C, so as to obtain 5-(methoxycarbonyl)-2-oxo-1, 3-dioxolane-4-methyl formate, namely the 5-(methoxycarbonyl)-2-oxo-1, 3-dioxolane-4-methyl formate, namely the 5-(methoxycarbonyl)-2-oxo-1, 3-dioxolane-4-methyl formate. After dropwise adding, heating to room temperature, stirring, and concentrating filtrate to obtain an intermediate; and 2, adding the intermediate, a second organic solvent, a catalyst and methanol into a reflux reaction container with a water knockout drum and a condenser, carrying out heating reflux reaction to separate water, concentrating the reaction liquid after the reaction is finished to obtain a crude product, adding the crude product into a first organic solvent, carrying out heating reflux, filtering to remove insoluble substances while the crude product is hot, cooling and crystallizing the filtrate, carrying out suction filtration, and drying to obtain the target product. The method has the advantages that the synthesis method is simple and easy to implement, the post-treatment method is easy to operate, and the product is high in purity and good in yield.

The invention discloses a preparation method of an antibacterial sleep-aiding latex pillow, and relates to the technical field of latex. Silicon dioxide is preliminarily modified through 4-trimethoxysilylbutyraldehyde, m-phenylenediamine-sodium sulfonate and triphosgene, the antibacterial and anti-dust effects can be achieved, then natural silk fibroin and collagen are used for further modification, performance is improved, meanwhile, the modified silicon dioxide can form a particle layer on the surface of natural latex, and the antibacterial and anti-dust effects are achieved. Modified silicon dioxide is used as a nucleating agent, and an interpenetrating network structure is formed through supercritical foaming, vulcanization, deblocking and crosslinking of the modified silicon dioxide and the nucleating agent, so that the mechanical property of the latex pillow is improved; according to the invention, after foaming, aromatic particles are doped, the sleep-aiding essential oil composition is fixedly loaded by using graphene aerogel microspheres, and cyclodextrin is used for encapsulation, so that the aromatic particles can release essential oil only when in use.

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.

The invention discloses a preparation method of 4, 6-dichloropyrimidine, and belongs to the field of organic synthesis, and the preparation method comprises the following steps: in the presence of an organic solvent or no solvent, mixing 4-chloro-6-methoxypyrimidine with DMF (Dimethyl Formamide), dropwise adding a chlorination reagent under a certain temperature condition, carrying out a heat preservation reaction, and then carrying out post-treatment to obtain the 4, 6-dichloropyrimidine. The preparation method is simple to operate, mild in condition and simple in post-treatment, and 4, 6-dichloropyrimidine can be prepared without using a phosphorus-containing reagent and a highly toxic reagent phosgene or triphosgene.

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 belongs to the technical field of fine chemical engineering, and particularly relates to an integrated process for continuously producing diphenylmethane diisocyanate (MDI) and a modified product thereof based on triphosgene (BTC). The invention discloses an HG catalyst which is prepared by adopting a compound template agent and combining a microwave-hydrothermal combined method with a supercritical CO2 drying technology. The invention further discloses a method for continuously preparing the diphenylmethane diisocyanate and the modified product of the diphenylmethane diisocyanate, which comprises the following steps: preparing Ph-Amine by taking formaldehyde and aniline as raw materials under the action of an HG catalyst; ph-Amine and BTC are used as raw materials to carry out a three-stage continuous isocyanate esterification reaction, and finally, pure MDI and mixed MDI are respectively obtained through solvent recovery and purification, and the mixed MDI is used for preparing modified MDI.

The present invention belongs to the technical field of fine chemical engineering, and particularly relates to an integrated process for continuously producing diphenylmethane diisocyanate (MDI) and its modified products based on triphosgene (BTC). The present invention discloses an HG catalyst, which is prepared by using a compound template agent through a combined microwave-hydrothermal method and supercritical CO2 drying technology. The present invention also simultaneously discloses a method for continuously preparing diphenylmethane diisocyanate and its modified products: using formaldehyde and aniline as raw materials, under the action of the HG catalyst, Ph-Amine is prepared; then, using Ph-Amine and BTC as raw materials for a three-stage continuous isocyanation reaction, and finally through solvent recovery and purification, pure MDI and mixed MDI are respectively obtained, and the mixed MDI is used to prepare modified MDI.

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.

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 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.

The invention discloses a high-purity preparation method of N, N '-carbonyldiimidazole by using solid triphosgene, and relates to the technical field of organic synthesis.The high-purity preparation method comprises the steps that S1, raw materials are pretreated, and a reaction system is built; s2, optimizing a reaction process; s3, by-product treatment and product separation; s4, performing post-treatment and quality monitoring on the product; and S5, product post-processing and quality monitoring. According to the method, by means of by-product treatment and product separation, residual raw materials can be neutralized, water-soluble impurities can be extracted and separated, the product is subjected to preliminary separation and refining, then elution, crystallization and purification treatment are conducted, different types of impurities are treated in each step, and the content of various impurities in the product is gradually reduced through multi-stage treatment; and finally, the high purity of the product is ensured, the high-purity preparation of N, N '-carbonyldiimidazole is realized, a real-time monitoring and fine tuning mechanism is established, the reaction process is more stable and controllable, and the production efficiency and the consistency of the product quality are improved.

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.

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.

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.

The invention provides a method for continuously producing clindamycin hydrochloride, which comprises the following steps of: 1, preparing a solution of triphosgene in DMF (Dimethyl Formamide), namely a solution A; 2, preparing a solution of lincomycin or hydrochloride thereof in chloroform, namely a solution B; step 3, pumping the solution A and the solution B into a reaction plate according to a certain flow velocity for reaction to obtain a reaction solution C; step 4, pumping the reaction liquid C into a reaction plate according to a certain flow velocity for reaction to obtain a reaction liquid D; 5, the reaction liquid D is subjected to aftertreatment, and clindamycin hydrochloride is obtained. The method is high in reaction conversion rate, few in side reaction impurities, safe in production and suitable for industrial production.

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.

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 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.

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 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.

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 discloses a dual-channel fluorescent probe for simultaneously detecting A beta and HClO / ClO-as well as a preparation method and application of the dual-channel fluorescent probe, and belongs to the technical field of fluorescent probes. The preparation method comprises the following steps: dissolving 4-(dimethylamino) phenylboronic acid and 4-bromo-2-hydroxybenzaldehyde in ethylene glycol dimethyl ether, adding tetrakis (triphenylphosphine) palladium and a sodium carbonate aqueous solution, reacting to obtain a compound 1, dissolving the compound 1 and monoethyl adipate in dichloromethane, and adding piperidine; reacting to obtain a compound 2; the preparation method comprises the following steps: dissolving methylene blue and sodium carbonate in water and dichloromethane, adding sodium thiosulfate, dropwise adding a dichloromethane solution of triphosgene, reacting to obtain a compound 3, dissolving the compound 3 and triethylamine in dichloromethane, adding 2-(4-aminophenyl) ethylamine, and reacting to obtain a compound 4; and dissolving the compound 2 in dichloromethane, adding DIPEA, HATU and a compound 4, and reacting to obtain the dual-channel fluorescent probe. The dual-channel fluorescent probe shows completely independent spectral response to A beta plaque and HClO / ClO-, and has high selectivity and sensitivity.

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.