10 results about "Chloracetone" patented technology

The application discloses a method for synthesizing benoxacor, and belongs to the technical field of chemical organic synthesis. The method comprises the following steps: taking DMF as a solvent, fully reacting ortho-nitrophenol with monochloroacetone and alkali at a certain temperature, centrifuging after the reaction is completed, obtaining a first filter cake and a DMF solution of 2-nitro-2-phenoxypropanone, removing part of the DMF through vacuum distillation, detecting the content of chloroacetone in the gas chromatograph, and adjusting the mass concentration of the 2-nitro-2-phenoxypropanone DMF solution to 10-20% after the content of chloroacetone is detected to be lower than 0.02% by using the area normalization method; then, adding Raney nickel into the 2-nitro-2-phenoxypropanone DMF solution, and performing hydrogenation reaction by passing hydrogen; after the reaction is completed, the upper clear liquid is extracted, and 3,4-dihydro-3-methyl-2H-1,4-benzoxazine DMF solution is obtained through filtration; then, an acid-binding agent alkali is added, and acylation reaction is performed by dropwise adding dichloroacetyl chloride, so as to synthesize benoxacor. The method can greatly simplify the operation process of frequently changing solvents in the process of synthesizing benoxacor, and can avoid the generation of a large amount of waste brine.

The invention relates to the technical field of refined reaction regulation and control of chloroacetone, in particular to an optimized regulation and control method for reaction preparation of chloroacetone, which comprises the following steps: S1, setting a regulation and control target and a reaction state judgment threshold value; s2, collecting reaction liquid detection data, and calculating to obtain the actually measured concentration of chloroacetone; s3, substituting into a chloroacetone concentration correction logarithmic model, and calculating to obtain the actual concentration of chloroacetone; s4, substituting the process adaptation type relative deviation into a chloroacetone reaction state entropy scoring model to obtain a comprehensive score and delimiting a reaction grade; s5, substituting into a chloroacetone chlorine flow dynamic regulation and control model, and calculating the chlorine flow regulation quantity; and S6, performing hierarchical regulation and control according to reaction grades to complete collection of the chloroacetone product. According to the invention, the core factors of the chloroacetone chlorination gas-liquid two-phase reaction are integrated to realize multi-dimensional cooperative regulation and control, so that the technical problems of regulation and control lag and process parameter imbalance in the traditional chloroacetone reaction regulation and control process are effectively solved, and the regulation and control accuracy and real-time response capability of the chloroacetone reaction are remarkably improved.

The invention provides a synthesis method of N-phenyl-N-benzyl-alanine acetone ester, which comprises the following steps: by taking N-phenylalanine and benzyl chloride as raw materials, carrying out substitution reaction under the catalysis of inorganic base to obtain an intermediate product N-phenyl-N-benzyl alanine sodium salt; and reacting the intermediate product with chloroacetone under the action of a phase transfer catalyst to obtain the N-phenyl-N-benzyl-alanine acetone ester product. According to the invention, a one-pot method is adopted for synthesis, and the steps of intermediate product separation, reaction container transfer and the like in the traditional process are omitted, so that the reaction process is simplified, the reaction efficiency is improved, the product waste can be reduced, the product yield and content are improved, the total molar yield is improved by more than 15% compared with the traditional mode, and the content is improved to more than 99% from the original 92%; according to the method, cheap chloroacetone is used as a raw material to replace the original expensive bromoacetone, so that the cost of the raw material is greatly reduced, and the economic benefit is improved.

The utility model relates to the field of trichloroacetone production, in particular to trichloroacetone production equipment. The trichloroacetone production equipment provided by the utility model has the beneficial effects that when a container filled with trichloroacetone is transported and protected, the container filled with the trichloroacetone is prevented from being damaged by splashing articles in a production workshop, so that the risk of carrying the trichloroacetone is reduced. According to the technical scheme, the trichloroacetone production equipment comprises a protection frame and a disc base fixedly connected to the bottom of the inner side of the protection frame, filling bottles are placed on the disc base, a plurality of sliding frames are evenly connected to the protection frame in the circumferential direction of the central axis of the disc base in a sliding mode, and the sliding frames are arranged on the disc base. And a clamping arc plate is fixedly connected to the position, located on the inner side of the protection frame, of each sliding frame, and the multiple clamping arc plates are attached to and clamped on the surface of a bottle body of the filling bottle in the circumferential direction.

The application provides a catalytic synthesis method of famotidine intermediate 1,3-dichloropropanone, the catalytic synthesis method is that a molecular sieve loaded phosphotungstic heteropoly acid catalyst is used as a catalyst of a reaction system of 1,3-dichloropropanol and hydrogen peroxide, the phosphotungstic heteropoly acid is a solid catalyst, but the specific surface area is small, by loading the phosphotungstic heteropoly acid on the molecular sieve, the phosphotungstic heteropoly acid can have the acid catalytic activity and the large specific surface area; in addition, the molecular sieve in the application can strengthen the carbonylation reaction activity in the reaction process, shorten the reaction time, the reaction can be carried out at a lower reaction temperature, the catalyst loss is reduced, the reaction process is simple, the operation is convenient, meanwhile, the yield of 1,3-dichloropropanone is high, the highest can reach 80%, and the application has a wide application prospect.

The invention discloses spherulitic cloxacillin sodium and a preparation method thereof, and belongs to the field of medicine synthesis. The spherocrystal is a spherical polycrystalline aggregate which is formed by radially growing towards each radial direction by taking a crystal nucleus as a center. The preparation method comprises the following steps: taking 6-APA, o-chloroacyl chloride and sodium isooctanoate as initial raw materials; the method comprises the following steps: adding water, NaOH and other solutions into 6-APA to form a 6-APA dissolving unit, then adding an o-chloroacyl chloride acetone solution to form an acylation unit solution, then adding dichloromethane, carrying out phase splitting, and then adding acetone into a lower layer phase to form an extraction unit solution; meanwhile, an acetone aqueous solution of sodium isooctanoate is used as a crystallization base solution. In the crystallization process, a part of the extraction unit solution is rapidly pre-added into a crystallization base solution, a seed crystal is added for pre-crystal growing, then the remaining extraction unit solution is added to complete a crystallization reaction and crystal growing, and the water mass is controlled to be 3%-8% in the crystallization process; and carrying out elution, filtration, washing and drying to obtain cloxacillin sodium spherulites. The method disclosed by the invention has the characteristics of easiness in suction filtration, low impurity content and high yield, and can obviously shorten the production period, improve the yield and improve the product quality.

The invention belongs to the field of fine chemical synthesis, and particularly relates to high-purity 1, 1, 1, 3-tetrachloroacetone as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) in the presence of a catalyst, contacting 1, 1, 1-trichloroacetone with chlorine for chlorination to obtain a 1, 1, 1, 3-tetrachloroacetone crude product; (2) carrying out reduced pressure distillation on the 1, 1, 1, 3-tetrachloroacetone crude product, and collecting a distillate of which the main fraction is 1, 1, 1, 3-tetrachloroacetone; (3) carrying out solvent crystallization on the distilled liquid by using water as a solvent, and washing to obtain a 1, 1, 1, 3-tetrachloroacetone hydrate crystal; and (4) carrying out rotary evaporation on the hydrate crystal to remove moisture. The method disclosed by the invention can be used for preparing a large amount of standard substances of the impurity 1, 1, 1, 3-tetrachloroacetone of the 1, 1, 3-trichloroacetone, and the purity can reach 95% or above; the method is simple, and the obtained high-purity product can be used as a standard substance to accurately and effectively detect the content of impurity 1, 1, 1, 3-tetrachloroacetone in 1, 1, 3-trichloroacetone.

The application relates to the technical field of organic synthesis, and discloses a method for continuously preparing folic acid through pipe reactor collision. High pressure of a pipe reactor is used to make sodium pyrosulfite and N-(4-aminobenzoyl)-L-glutamic acid and 2,4,5-triamino-6-hydroxypyrimidine sulfate homogeneously disperse, raw materials are fully dispersed under the condition of less aqueous solvent, high-speed flow generated by high pressure is used to make N-(4-aminobenzoyl)-L-glutamic acid, 2,4,5-triamino-6-hydroxypyrimidine sulfate and trichloroacetone collide to occur a cyclization reaction, and the problem that material reaction is insufficient due to folic acid deposition and wrapping is avoided; sodium carbonate solution is sprayed to the continuous collision liquid flow, loss of raw materials caused by local alkali hydrolysis of trichloroacetone is avoided, the purity and yield of folic acid crude product are significantly improved, and the amount of waste water is reduced. The whole preparation process is a closed pipeline and a closed container, odor volatilization is avoided to affect the operation space, automatic control is easy, and the method is suitable for industrial production.

The utility model discloses a device for recovering chloroacetone in waste water in the chloroacetone production process, which belongs to the field of chloroacetone recovery and comprises a shell, a first barrel and a second barrel are arranged in the shell and communicated through a connecting pipe, the top of the first barrel and the top of the second barrel are both connected with a motor, and the first barrel and the second barrel are arranged in the shell. And the output end of the motor is connected with a stirring rod. Through arrangement of a stirring rod, a cleaning assembly and a motor, during use, the motor is started to drive the stirring rod to rotate, the stirring rod rotates to drive rotating frames on the two sides to rotate, cleaning rollers are tightly attached to the inner wall of a barrel under the action of springs when the rotating frames rotate, and then the cleaning rollers are driven to rotate with the stirring rod as the center; and meanwhile, when the cleaning roller rotates for cleaning, the cleaning roller makes contact with the inner wall of the barrel to drive the cleaning roller to rotate, the medium on the inner wall of the barrel is further cleaned, and therefore the cleaning effect is improved.

The utility model discloses a wastewater treatment device in a chloroacetone production process, which belongs to the technical field of chloroacetone production processes and comprises an extraction tower component and a rectifying tower component. According to the utility model, the chloroacetone in the wastewater is recovered through extraction and rectification technologies, and the design that the distribution coefficient of the chloroacetone in an extraction agent is large is utilized, so that the recovery efficiency of the chloroacetone is effectively improved, the chloroacetone in the wastewater can be efficiently recovered, the product loss is reduced, the smooth discharge of water is ensured, and the device is reasonable in design, simple and convenient to operate and low in cost. The cost is low, the environment-friendly effect is good, the conditions of resource waste and environment pollution are avoided, and wide industrial application prospects are achieved.