27 results about "Ketone synthesis" patented technology

The synthesis process comprises the following steps: (1) introducing inert gas into a reactor, adding a solvent, a Lewis acid catalyst and diphenyl ether, then dropwise adding an acyl chloride monomer solution, and synthesizing an intermediate M with a short-chain small molecular structure; (2) continuously dropwise adding an acyl chloride monomer solution into the reactor for reaction, and then adding an end-capping reagent for reaction; and (3) quenching, washing and drying the reaction product in the step (2) to obtain the product. Under the condition that only the Lewis acid is used as the catalyst, the one-pot method is adopted for synthesizing PEKK in two steps, side reactions can be reduced, meanwhile, the dosage of the catalyst is reduced, the production cost is reduced, the post-treatment process is simplified, and the obtained polyether ketone ketone is high in molecular weight and good in heat resistance and mechanical performance.

The invention relates to a method for synthesizing an iodo-pyridine compound from N-propargyl enaminone, which comprises the following steps: by taking N-propargyl enaminone as a raw material, DMF (Dimethyl Formamide) as a reaction solvent and copper acetate and N-iodosuccinimide as accelerators, carrying out intramolecular coupling reaction at 60 DEG C to synthesize the iodo-pyridine compound. The method for directly synthesizing the pyridine heterocyclic compound through the intramolecular coupling reaction of the N-propargyl enaminone under the non-alkaline condition is disclosed for the first time, reaction substrates are not limited to benzene rings on alkynyl, the application range of the reaction is greatly expanded, and the method has the advantages of being wide in substrate range, strong in functional group application range, mild in reaction condition, easy to operate, safe, high in yield and the like. And raw materials are cheap.

The invention discloses a synthetic carbamate compound based on 3-substituted dioxazolone as well as a preparation method and application of the synthetic carbamate compound, and belongs to the technical field of organic synthesis. The synthesis method comprises the following steps: (1) preparing 3-substituted dioxazolone from hydroximic acid with different substituent groups and phosgene under an ice bath condition; and (2) reacting the 3-substituted dioxazolone obtained in the step (1) with different phenols (alcohols) under an alkaline condition to obtain corresponding carbamate compounds. According to the method, the yield of carbamate is further improved by adjusting the conditions of alkali, equivalent weight, temperature and the like; the preparation method provided by the invention is novel and has the advantages of mild reaction conditions, few generated impurities, high yield, high safety, convenience in operation and the like; and the compound shows good cholinesterase activity in activity screening, and can be used in insecticides or pesticides.

The utility model relates to the technical field of synthesis of methyl isobutyl ketone, and discloses a feeding device for synthesis of methyl isobutyl ketone, which comprises a main body mechanism and a quantifying mechanism and is used for conveying metered materials to a processing area. According to the feeding device for synthesis of methyl isobutyl ketone, the feeding port and the conveying pipe are arranged on the feeding bin, liquid, solid and gas materials can be added at the same time, various process requirements are met, the pressure gauge and the pressure sensor are further arranged at the upper end of the feeding bin, the pressure change in the bin can be monitored in real time, and the safety and stability of the operation process are ensured; the metering hopper is connected with the feeding bin and the discharging pipe through hoses, mobility is provided, the weighing process is prevented from being affected by fixed connection, the hoses are fixed to all parts through pipe hoops, firmness and sealing performance of connection are guaranteed, and the weighing device is suitable for long-time operation.

The invention discloses a peach ketone synthesis method, which relates to the technical field of essence and perfume synthesis, and comprises the following steps: adding cyclopentanone and glacial acetic acid into a reaction container, starting stirring, adding manganese acetate (II) and cobalt acetate (II), and then adding acetic anhydride; introducing dried air below the liquid level, heating to 80-100 DEG C, dropwise adding D-limonene, and carrying out a heat preservation reaction after dropwise adding is finished; gC monitors the reaction endpoint, and the reaction is stopped when the product purity of the reaction liquid is not increased any more; after the reaction is finished, filtering, carrying out reduced pressure distillation to recover cyclopentanone, glacial acetic acid and unreacted D-limonene, after the recovery is finished, adding methanol and n-heptane into kettle liquid, carrying out water extraction, washing and liquid separation, washing an organic phase with a sodium bicarbonate aqueous solution, carrying out reduced pressure distillation on the organic phase to recover n-heptane, and after the recovery is finished, obtaining a peach ketone crude product; and carrying out crude drawing and rectification on the peach ketone crude product to obtain a peach ketone finished product. The method has the advantages of mild reaction conditions, low safety risk and few three wastes, and can obtain a high-purity peach ketone finished product.

The invention discloses a novel process for synthesizing N-vinyl pyrrolidone, and provides a preparation method of N-vinyl pyrrolidone, which is efficient, low in cost and energy-saving. Raw materials of alpha-pyrrolidone and a catalyst potassium salt react in a high-vacuum reactive distillation tower, the reaction temperature is controlled, the reaction product water is distilled out from the tower top, and the generated alpha-pyrrolidone potassium salt is buffered by a buffer tank and then sent to an N-vinyl pyrrolidone reactor. In order to ensure the stable supply of acetylene in the synthesis reaction of N-vinyl pyrrolidone, a method of supplementing nitrogen with a surge tank is adopted to maintain the stability of the system. And carrying out low-pressure flash evaporation on the reacted N-vinyl pyrrolidone gas-liquid product through a surge tank, recycling the gas phase, and obtaining the N-vinyl pyrrolidone crude product from the liquid phase. According to the process, the conversion per pass of the alpha-pyrrolidone can reach 55%, the purity of the N-vinyl pyrrolidone is greater than or equal to 98%, and the energy consumption is reduced by 20%.

The invention relates to the technical field of perfume synthesis, in particular to an efficient hydrolysis process in perfume synthesis, which comprises the following steps: mixing ethyl lactate, ethyl 3-chloropropionate and ethanol, and reacting under the conditions of metal sodium and heating reflux; after the reaction is finished, distilling off the ethanol under reduced pressure, neutralizing the residual reaction liquid with dilute sulphuric acid, extracting with an organic solvent, separating the liquid to obtain an organic phase, and concentrating the organic phase under reduced pressure to obtain a 2-methyl-4-methyl ester tetrahydrofuran-3-ketone crude product; the method comprises the following steps: heating a 2-methyl-4-methyl ester tetrahydrofuran-3-ketone crude product under the catalysis of cationic resin to hydrolyze, filtering out the cationic resin, extracting with an organic solvent, separating liquid to obtain an organic phase, concentrating under reduced pressure, and rectifying to obtain breadone. According to the method for synthesizing breadone, use of a large amount of acid water is avoided, output of a large amount of waste acid is avoided, the process is more environmentally friendly, meanwhile, the yield is high, the steps are simple, and the industrial production prospect is wide.

The application discloses a green process for synthesizing 4-methyl-2H-pyrane-2,6(3H)-dione, which comprises the following steps: (a) hydrolyzing 4,6-dimethyl-2-oxo-2H-pyrane-5-ethyl formate with liquid alkali to obtain a hydrolysis mixture, and performing negative pressure distillation on the hydrolysis mixture to recover an ethanol aqueous solution; (b) neutralizing the product of the negative pressure distillation to 7.0-7.5, centrifuging to obtain a filtrate and a residue, drying the residue to obtain anhydrous sodium salt, and performing three-stage extraction on the filtrate to obtain an aqueous phase and an organic phase; (c) performing cooling crystallization on the aqueous phase, centrifuging to obtain a precipitate and a first centrifugal filtrate, wherein the first centrifugal filtrate is used for preparing liquid alkali; performing concentration crystallization on the organic phase, recovering an extraction agent, cooling to crystallize when the concentration crystallization is performed to the point that crystals are precipitated, and centrifuging to obtain 3-methyl pentene diacid solid and a second centrifugal filtrate, wherein the second centrifugal filtrate is used for concentration crystallization; and (d) performing ring formation on the 3-methyl pentene diacid by dehydration reaction with a dehydrating agent, wherein the dehydrating agent is acetic anhydride or acetyl chloride. In this way, the discharge amount of pollutants is greatly reduced.

The invention provides a piperidone synthesis tail gas treatment method, which comprises: (1) carrying out first condensation on piperidone synthesis tail gas to obtain a first condensate and a first non-condensable gas; performing second condensation on the first non-condensable gas to obtain second condensate and second non-condensable gas; recovering the first condensate and the second condensate with acetone to obtain an acetone product; (2) the second non-condensable gas is subjected to acid pickling absorption, and an absorption rich solution and absorption tail gas are obtained; crystallizing the absorption rich solution to obtain an ammonium salt product; and (3) sequentially carrying out water washing, third condensation and adsorption on the absorption tail gas to obtain purified gas. The method provided by the invention can realize recovery of acetone and resource utilization of ammonium sulfate by-products, and has a wide application prospect.

The utility model provides a kind of for ringazine ketone synthesis automatic mixing device, belong to ringazine ketone synthesis technical field, including mounting plate, mixing box and mounting frame, the top of mounting plate is fixedly installed with mounting sleeve, the inside sliding installation of mounting sleeve has sliding rod, the top of sliding rod is fixedly installed with first motor.The utility model can make gear rotate by the rotating action of second motor output end, meshing between gear and rack is utilized, so that sliding rod can slide along the inside of mounting plate, so that rotating shaft can be in the process of descending can make protective cover and the top of mounting plate adhere to each other, while rotating shaft moves up and down in the process, can drive stirring vane moves up and down in the inside of mounting plate, can be more uniform in the process of mixing, so that buffer sleeve and mixing box adhere to each other limit, buffer sleeve and the outside of mixing box can be closely adhered to each other by spring.

The utility model relates to the technical field of material filling, and discloses a feeding device for synthesis of methyl isobutyl ketone, which comprises a tank body, a cleaning mechanism, a feeding pipe, a discharging port, a feeding pipe, a feeding pipe, a discharging port, a feeding mechanism, a feeding mechanism, a discharging mechanism and a discharging mechanism, and is characterized in that the top of the tank body is fixedly connected with a top plate, and the top of the top plate is fixedly connected with the feeding pipe; the cleaning mechanism comprises a servo motor fixedly connected to the top of the top plate, the output end of the servo motor is fixedly connected with a transmission rod, and a scraper is arranged outside the transmission rod. The adjusting mechanism comprises an adjusting shell fixedly connected to the outer portion of the discharging port, the worm is driven by the rotating disc to rotate, so that the worm gear is driven to rotate, finally the adjusting plate is made to rotate, materials are smoothly discharged through linkage operation of a series of structures, and the discharging efficiency is improved. The feeding amount during synthesis of methyl isobutyl ketone can be accurately controlled, it is ensured that the synthesis reaction is carried out according to expectation, and the accuracy and stability of the synthesis reaction are improved.

The invention belongs to the field of molecular biology and enzyme engineering, and discloses an amine dehydrogenase mutant and application thereof in chiral beta-aminoketone synthesis. The amine dehydrogenase mutant provided by the invention can catalyze reductive amination of various 1, 3-diketone substrates, the substrate spectrum of the mutant is greatly broadened, the activity of the amine dehydrogenase in catalytic synthesis of chiral beta-aminoketone is remarkably improved, the problems of low activity, poor regioselectivity, narrow catalytic substrate range and the like of the amine dehydrogenase are solved, and the application prospect is broad. Wide application prospects are realized.

The invention belongs to the field of organic synthesis and catalysis, and particularly relates to a method for synthesizing damascenone B. According to the method, narrow-pore sulfonic acid type polystyrene-divinylbenzene supported acid resin A1-M1 is adopted as a catalyst, beta-ionone isomerization rearrangement is catalyzed in a mixed solvent of ethyl alcohol and 2-methyltetrahydrofuran, the content of water in a reaction system is accurately controlled to be 0.01-0.10 wt%, generated water is continuously removed, and the content of the water in the reaction system is accurately controlled to be 0.01-0.10 wt% in combination with the narrow-pore confinement effect of the catalyst, so that beta-ionone isomerization rearrangement is achieved. The high-selectivity synthesis of the damascenone B is realized. The organic purity of the product is 99.2-99.9 wt%, the isomer selectivity is 97.0-99.5 wt%, the residual solvent is less than or equal to 1000mg / kg, and the heavy metal content meets the essence raw material standard. The problems that in the prior art, mechanical stability and multi-cycle usability of a catalyst are difficult to consider, extremely low water content control and catalytic activity are kept contradictory, deep purification of products and mild operation conditions conflict and the like are solved, and the industrial application value of flavors and fragrances is wide.

The application discloses a watermelon ketone synthesis production process organic waste gas treatment device, belongs to the field of waste gas treatment. The watermelon ketone synthesis production process organic waste gas treatment device, including main body cylinder, air inlet bin and air outlet bin, the side of air inlet bin is equipped with waste gas treatment main part, the side of air inlet bin is equipped with cleaning brush frame driven by linear motor, the inside of main body cylinder is equipped with fixed plate. The watermelon ketone synthesis production process organic waste gas treatment device, start suction fan and cleaning brush frame, the suction fan in rotating state can drive the sleeve transmission connection fast rotation, cooperate with moving block one, spring one, arc plate, torsional spring block one, rotating rod one, rotating rod two, moving rod one, spring two and stress plate, so that the cleaning brush frame is moved and receives additional force, so as to improve the friction between the cleaning brush frame and the waste gas treatment main part, improve the cleaning effect of the cleaning brush frame.

The invention provides a synthetic method of methyl cyclopentenolone, and belongs to the technical field of organic synthesis. In the synthesis process, a proper amount of copper-nickel alloy catalyst is added in the rearrangement synthesis section to catalyze the reaction, and after a rearrangement extraction agent is changed from methylbenzene to p-xylene, under the same feeding proportion, the overall yield of methyl cyclopentenolone synthesis is increased by about 10% by using the catalyst and the p-xylene extraction process compared with a conventional process.

The invention relates to the technical field of polyether ketone synthesis, in particular to a polyether ketone synthesis reaction device and a using method thereof.The polyether ketone synthesis reaction device comprises a closed reaction kettle body, a stirring motor, a connecting flange and a mounting window, and the mounting window is formed in the upper end of the closed reaction kettle body; a stirring motor is fixedly connected to the upper end of the mounting window through a connecting flange, a sealing ring and bolts, a stirring shaft is fixedly connected to the top end of a main shaft of the stirring motor, stirring blades are mounted at the lower end of the stirring shaft, and adjusting units are mounted at the lower ends of the stirring blades; the stirring shaft comprises a circular shaft, inclined grooves are formed in the two sides of the lower end of the circular shaft, high-temperature-resistant telescopic sealing pieces are installed in the inclined grooves, and a high-temperature-resistant spring and a jacking column are fixedly connected into the circular shaft; in the invention, a purely mechanical and self-adaptive regulation and control stirring scheme is provided, and the phase change characteristic of the shape memory alloy material is utilized, so that the form of the stirring paddle and the stirring mode can be accurately and automatically matched with the viscosity-temperature characteristics of different stages of the polyetherketoneketone synthesis reaction without delay.

The invention provides a preparation method of 6-hydroxy-4-chloro-2-ethyl-6H-pyran-3-ketone, which comprises the following steps: S1) mixing furfuryl propanol with a solution of an inorganic alkaline compound to carry out first reaction to obtain a first solution; s2) carrying out a second reaction on the first solution and chlorine to obtain a second solution; and S3) performing separation and purification on the second solution to obtain the 6-hydroxy-4-chloro-2-ethyl-6H-pyran-3-one. The invention also discloses a preparation method of the 6-hydroxy-4-chloro-2-ethyl-6H-pyran-3-one. The synthesis method can be used for solving the problem of low purity of 6-hydroxy-4-chloro-2-ethyl-6H-pyran-3-ketone synthesized by a synthesis method in the prior art, and is suitable for the field of synthesis of 6-hydroxy-4-chloro-2-ethyl-6H-pyran-3-ketone.

The application relates to the technical field of reaction kettle equipment, and discloses a cyclization reaction kettle for furanone synthesis and a processing method thereof. External medium is supplied into a heating cavity, part of raw materials in a reaction cavity is rapidly heated through the heating cavity, the heated raw materials are injected into the reaction cavity, the uniform heating rate is accelerated, the external raw materials are injected into the middle part of the reaction cavity, the mixing between materials is further accelerated, at the same time, a grinding head moving up and down and rotating along with a power fan is arranged in the reaction cavity, the existence of the agglomerated materials in the reaction cavity is crushed when the grinding head moves downward, and the effects of accelerated mixing and heating and material crushing are finally realized.

The invention provides a simple and efficient synthesis method, in particular to a method for realizing insertion of a formyl compound C-H into intramolecular olefin to construct an indolone compound containing a chiral quaternary carbon center by connecting a phosphorus-oxygen ligand with a nickel-aluminum bimetallic catalyst, and belongs to the technical field of methodology development. The key of the problem solved by the invention is as follows: 1, a formyl compound which is efficient and specific in reaction activity and site selectivity is found; 2, a bimetallic catalytic system is designed by utilizing the characteristics of phosphine oxide ligands, so that the reaction enantioselectivity is greatly improved;

The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing bicyclo [1.1. 1] pentane benzyl alcohol, which comprises the following steps: by taking aromatic aldehyde, [1.1. 1] propeller alkane and a dihydroquinazoline derivative synthesized by ketone as initial raw materials and dichloroethane and the like as a solvent, carrying out three-component free radical coupling reaction under the protection of inert gas and under the illumination condition to obtain the bicyclo [1.1. 1] pentane benzyl alcohol. And a bicyclo [1.1. 1] pentane benzyl alcohol product is synthesized in one step. The method has the advantages of mild reaction conditions, high reaction efficiency, low cost, simplicity and convenience in operation and the like, and a new method is provided for later structural modification of diaryl methanol drug molecules.

The invention discloses an efficient and green synthesis method of benzodifuran diketone, and belongs to the field of conductive polymer synthesis. The method comprises the following steps: by taking hydroquinone as a basic raw material, firstly, carrying out esterification reaction on hydroquinone and chloroacetyl chloride under the action of an alkaline compound to produce an intermediate 1, 4-phenylene bis (2-chloracetate); and then carrying out Friedel-Crafts reaction on the intermediate under the catalytic action of acid, or catalyzing by palladium metal and carrying out self-cyclization reaction to generate the benzodifuran diketone. According to the invention, a stable, efficient and green benzodifuran diketone synthesis process is established, the generation of byproducts is effectively controlled while high yield is realized, and the product is easy to purify. Compared with the traditional method, the synthesis steps are greatly reduced, the raw material source is wide, the reaction condition is mild, the operation is safe, the overall cost is obviously reduced, the method is suitable for large-scale batch production, and guarantee is provided for stable supply, high conductivity and other properties of the polybenzodifuran diketone material; and an important foundation is laid for a next-generation high-performance and sustainable organic electronic material system.

The application provides a method for synthesizing damascenone from 6-methyl-3-heptene-2-ketone, which comprises the following steps: S1, 6-methyl-3-heptene-2-ketone and a methyl metal reagent are subjected to addition reaction to obtain a 2,6-dimethyl-3-heptene-2-ol intermediate; and S2, the 2,6-dimethyl-3-heptene-2-ol is subjected to hydrogenation reaction to obtain a damascenone product. The synthesis route is short and novel, and the damascenone product is prepared in a simple and efficient manner from 6-methyl-3-heptene-2-ketone which is cheap and easy to obtain through two-step addition and reduction reaction, and the overall yield of the route is high. Compared with the traditional process using 6-methyl-5-heptene-2-ketone, the raw material cost is significantly reduced. In addition, it is found that the addition of a trace amount of tertiary carbonic acid in the hydrogenation reaction liquid can improve the selectivity of the target product damascenone.

The invention belongs to the technical field of green chemistry, and particularly relates to a method for bi-directionally synthesizing chiral lactam through bi-enzyme cascade-chemical catalysis. According to a methylpiperidone synthesis route taking 2-methyl glutaronitrile as a raw material, nitrile hydratase is subjected to iterative saturated mutation, substrate channel residues and active site residues are subjected to semi-rational engineering transformation, and 4-cyano valeramide and 4-cyano-2-methyl butyramide are generated with high selectivity. And carrying out cascade reaction on the modified nitrile hydratase and amidase, so as to directionally generate the corresponding mono-cyano carboxylic acid. Then, a Raney nickel catalyst hydrogenation reaction is adopted to treat the whole-cell catalytic solution, and two regioselectivity products can be obtained, namely 5-methyl-2-piperidone (the yield is 96.9%, and the regioselectivity is 98.3%) and 3-methyl-2-piperidone (the yield is 67.9%, and the regioselectivity is 70.4%).

The application discloses a kind of ( R )‑4‑isopropyl‑3‑(( R )‑2‑methyl‑5‑hexenoyl) oxazolidine‑2‑ketone and application in synthesis western hemlock looper sex pheromone component, it relates to the technical field of biological pesticide.The application utilizes ( R )‑4‑isopropyl‑3‑(( R )‑2‑methyl‑5‑hexenoyl) oxazolidine‑2‑ketone synthesis (5 R ,11 S )‑5,11‑dimethyl heptadecane, total yield can reach 18%, and (5 R ,11 S )‑5,11‑dimethyl heptadecane optical purity is greater than 99%;The application utilizes ( R )‑4‑isopropyl‑3‑(( R )‑2‑methyl‑5‑hexenoyl) oxazolidine‑2‑ketone synthesis ( S )‑7‑methyl heptadecane, total yield can reach 30%, and (5 R ,11 S )‑5,11‑dimethyl heptadecane optical purity is greater than 99%.

The utility model relates to the technical field of quinclorac-oxadiazon synthesis appliances, in particular to a water bath heating device for quinclorac-oxadiazon synthesis, which comprises a heating box body, a cover body, a water bath heating device, a water bath heating device and a water bath heating device, the lifting assembly is arranged on the cover body and comprises a supporting frame, the supporting frame is in threaded connection with the interior of a screw hole in a rotary disc, the rotary disc is rotationally connected to the cover body, the rotary disc is connected with a driving part, and a limiting rod used for limiting rotation of the supporting frame is further arranged on the cover body. By arranging the lifting assembly, a container containing a reaction solution is placed on the supporting frame, when the supporting frame is located in the heating box body, rapid water bath heating is conducted on the container, when the reaction tends to be finished, the driving piece drives the rotating disc to rotate, and due to the fact that the supporting frame is limited by the limiting rod, the rotating disc rotates to drive the supporting frame to ascend; therefore, the reaction condition at the bottom of the container can be observed visually, operation is simple, and safety is high.

The application provides a preparation method of dextromethorphan, which comprises the following steps: taking cyclohexanedione 1 as a raw material, and performing an acetonitrile group substitution reaction to obtain compound 2; performing a Villier-Michel ketone synthesis reaction on the compound 2 to obtain compound 4; performing a ketal protection on the compound 4 to obtain compound 5; performing a Robinson ring expansion reaction on the compound 5 to obtain compound 6; performing an aromatization reaction and a methylation reaction on the compound 6 to obtain compound 7; performing a ketone group deprotection on the compound 7 to obtain compound 8; performing a double bond isomerization reaction on the compound 8 to obtain compound 9; performing an acetonitrile group reduction reaction on the compound 9 to obtain compound 10; performing a lactam cyclization reaction on the compound 10 to obtain compound 11; and performing an asymmetric hydrogenation reaction on the compound 11 to obtain dextromethorphan. The application develops a new asymmetric synthesis route for preparing dextromethorphan, avoids intermediate resolution, and improves the yield.

The application discloses a synthesis method of 2,2,6,6-tetramethyl-4-piperidone, and belongs to the technical field of 2,2,6,6-tetramethyl-4-piperidone synthesis. The method adopts a synthesis system comprising a gas-liquid-solid three-phase reactor to prepare 2,2,6,6-tetramethyl-4-piperidone; the three-phase reactor is provided with a gas distributor at the bottom and is provided with a first material inlet and a second material inlet, the first material inlet is connected with the gas distributor, and the second material inlet is located below the gas distributor; a catalyst overflow outlet is arranged at the upper portion of the gas-liquid-solid three-phase reactor; raw material ammonia entering from the first material inlet is distributed through the gas distributor and reacts with raw material acetone entering from the second material inlet under the action of a catalyst, and the catalyst is discharged from the catalyst overflow outlet. The synthesis method has the technical advantages of simple and easy-to-control reaction process, low catalyst unit consumption, high ammonia conversion rate and selectivity, and low tail gas ammonia content.