90 results about "Ketone synthesis" patented technology

The invention discloses a polymer photocatalyst and a method of water-phase photo-catalytic selective alcohol oxidation. According to the invention, an organic polymer carbon nitride catalyst is prepared, and is applied in a water-phase photo-catalytic selective alcohol oxidation system. Compared with common ultraviolet catalyst TiO2, visible light catalyst TiO2-xNx, metal sulfide, metal nitride, metal nitrogen oxides, and the like, when alcohol is oxidized in water phase with a green oxidant air / oxygen under mild conditions, the carbon nitride catalyst is more stable and shows higher efficiency. The preparation method of the carbon nitride catalyst is simple and feasible, and the catalyst comprises no metal element, such that the catalyst is cheap. With the catalyst, alcohol oxidation aldehyde synthesis or ketone synthesis processes are simple and feasible, such that industrialized large-batch productions of aldehyde and ketone compounds can be facilitated.

The invention relates to a process method for synthesizing 1, 2-benzisothiazdin-3-ketone, which includes the steps: 1 enabling 2-chlorobenzonitrile and anhydrous sodium sulfide to react, and then performing acidification to obtain o-mercaptobenzonitrile; and 2 enabling the o-mercaptobenzonitrile to react with chlorine and water, cooling, crystallizing and obtaining target products. The process method adopts a 1, 2-benzisothiazdin-3-ketone synthesis method which is completely different from a traditional way, thereby greatly simplifying synthesis steps, lowering cost and reducing environment pollution simultaneously.

The invention relates to a synthesis method of a photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone, which comprises the following steps: reacting high-purity gas phosgene with isobutyric acid to synthesize isobutyryl chloride; and carrying out chlorine substitution reaction by a cascade technique: exhaust of a first reaction kettle after chlorine introduction is connected into a second reaction kettle in cascade, and hydrogen chloride and chlorine in the exhaust released by the first reaction enter the second reaction kettle to catalyze the absorption and utilization. The method can well enhance the purity of isobutyryl chloride and further enhance the purity and yield of the product 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone; and the catalytic action of hydrogen chloride in the exhaust is utilized to increase the reaction speed, lower the chlorine consumption and enhance the product content. The generated exhaust is recycled after innocent treatment, thereby solving the problem of environmental pollution of the exhaust.

The invention relates to the field of synthesizing N-vinyl pyrrolidone (NVP). A novel process is provided by the invention to realize safety usage of acetylene gas during synthesizing of the N-vinyl pyrrolidone (NVP). A novel tubular type reactor is employed to stably control the reaction temperature and prevent the generation of overtemperature side reactions. Nitrogen is employed to keep the pressure of a pressure control tank, and the pressure of the tubular type reactor is stabilized by the liquid level of the pressure control tank, so as to ensure that the acetylene is subjected to a continuous liquid phase reaction in the reactor. By employing a one-level tubular type reactor or multi-level tubular type reactors in series, the synthesis conversion rate of the N-vinyl pyrrolidone can reach to 20-80%, and selectivity reach to 95%.

Provided herein are methods for preparing ketone-containing organic molecules. The methods are based on novel iron / copper-mediated (“Fe / Cu-mediated”) coupling reactions. The Fe / Cu-mediated coupling reaction can be used in the preparation of complex molecules, such as halichondrins and analogs thereof. In particular, the Fe / Cu-mediated ketolization reactions described herein are useful in the preparation of intermediates en route to halichondrins.

The invention discloses a method for synthesizing progesterone. The method comprises the following steps: S1, performing synthesis of a compound 2: taking a derivative of 4AD as a raw material, takinga derivative of 4AD as a compound 1, taking chloroalkane as a solvent, adding an aqueous solution of tetramethylpiperidine oxide, sodium bromide and sodium bicarbonate, and carrying out oxidation reaction with a sodium hypochlorite solution to obtain the compound 2; S2, synthesizing a compound 3, namely reacting the compound 2 with 1-(1-piperidyl) cyclohexene under the protection of nitrogen by taking acetonitrile as a solvent to obtain a compound 3; S3, performing synthesis of progesterone: taking chloroalkane as a solvent of the compound 3, adding a dimethylformamide solvent for dissolvingcuprous chloride, and carrying out post-treatment to obtain progesterone; and S4, performing purification of progesterone: refining and purifying progesterone by using dichloromethane and sodium hypochlorite. The invention mainly aims at a progesterone synthesis method, and the synthesis route has the advantages of cheap initial raw materials, simple reaction steps, mild reaction conditions, economy, environmental protection, and suitableness for industrial implementation.

The invention relates to a preparation method of watermelon ketone, which comprises the following steps: by taking 4-methylcatechol and 1,3-dichloroacetone as raw materials and carbonate as a base catalyst, adding a drying agent into a Soxhlet extractor for dehydration, and under the protection of inert gas, assembling a reduced pressure reflux water removal device to prepare a watermelon ketone crude product; carrying out rotary evaporation to recover a solvent, carrying out post-treatment steps of decoloration, concentration and the like, and transferring an obtained solution into a rectification device provided with a glass vacuum rectification column to carry out segmented rectification: in first-stage rectification, evaporating off reaction solvent light components, in second-stage rectification, collecting fractions to obtain a residual raw material 4-methylcatechol and a part of crude product watermelon ketone, and in third-stage rectification, collecting a main fraction watermelon ketone crude product; and recrystallizing the watermelon ketone crude product. According to the preparation method of the watermelon ketone, the yield of the watermelon ketone is improved through the reduced pressure reflux water removal device, the watermelon ketone is purified step by step by combining segmented rectification and recrystallization, the purity of the product reaches 98% or above, the technological process is simplified, and the problem that industrial large-scale production is difficult to achieve through an existing watermelon ketone synthesis technology is solved.

The invention relates to an improved method for synthesizing clethodim. The method includes the step that propanoic acid C1-C6 alkyl ester is added into any procedure in the first step of reaction of a synthetic route shown in the formula (1). The formula (1) is defined in the description.

The invention relates to a method for synthesizing methyl cyclopentadiene from 3-methyl-2-cyclopentene-1-one. The method comprises the following steps: carrying out a hydrodeoxygenation reaction in afixed bed continuous reactor under the action of a supported metal oxide A / X catalyst by using 3-methyl-2-cyclopentene-1-one as a raw material to synthesize the target product methyl cyclopentadiene.The method is simple in process route, environmentally friendly and simple in catalyst preparation, and provides a new effective way for synthesis of methylcyclopentadiene from 3-methyl-2-cyclopentene-1-one.

The invention discloses a pyrazole ketone synthesis crystal kettle which comprises a cylinder, a feeding pipe and discharging pipe. A crystal chamber is formed in the cylinder, arc-shaped flow retaining plates are arranged on the inner walls of two sides of the crystal chamber, a mixing motor is arranged at the top end of the cylinder, a rotating shaft of the mixing motor extends to the bottom of the crystal chamber and does not contact with the bottom of the crystal chamber, an anchored mixing propeller is mounted at the bottom end of the rotating shaft, a cooling water circulation pipe is arranged in a cavity in the upper end between the crystal chamber and the cylinder, a plurality of nozzles are distributed on the cooling water circulation pipe, and the other end of the cooling water circulation pipe is connected with a water storage tank. The pyrazole ketone synthesis crystal kettle is high in cooling efficiency and fine in crystal effect, and cooling uniformity and crystal uniformity of materials are improved.

The invention discloses a ketone synthesis method through alkyne hydrolysis. The method comprises the following steps: adding alkyne, a catalyst [(IPr)AuCl], a solvent methanol, and water into a reactor, carrying out reactions for several hours at a temperature of 110 to 120 DEG C, cooling to the room temperature, carrying out rotary evaporation to remove the solvent, and performing column separation to obtain target compounds. Compared with conventional ionic gold catalyst, the provided method directly uses gold chloride [(IPr)AuCl] as the catalyst, alkyne is hydrolyzed into ketone, the yield is high, the selectivity is complete, and thus the method has an important meaning for organic synthesis and environment protection.

The invention aims to solve the technical problems of an existing alpha-hydroxycyclohexyl phenyl ketone synthesis method, provides a synthesis method of a photoinitiator 1-hydroxycyclohexyl phenyl ketone, and belongs to the technical field of chemical synthesis. The synthesis method comprises the following steps: (1) reacting a halogenated benzene with magnesium particles to prepare a Grignard reagent, dropwise adding cyclohexylcarbonitrile into the prepared Grignard reagent, and after the reaction is completed, hydrolyzing to generate cyclohexyl phenyl ketone; and (2) reacting cyclohexyl phenyl ketone with chlorine to obtain 1-chlorocyclohexyl phenyl ketone, and carrying out a hydrolysis reaction on the 1-chlorocyclohexyl phenyl ketone and a sodium hydroxide aqueous solution under the action of a catalyst to obtain 1-hydroxycyclohexyl phenyl ketone. The method is simple in synthesis process, high in yield and suitable for industrial production.

The invention discloses a photoresist resin monomer synthesized from spiro[2.5] decane-6, 8-diketone and a synthesis method of the photoresist resin monomer, which belongs to the technical field of chemical synthesis and photoetching. The structural general formula of the photoresist resin monomer is shown as a formula I, in the formula I, R1 is hydrogen or methyl; R2 is saturated alkane or cycloalkane; the synthesis method of the spiro [2.5] decane-6, 8-diketone compound comprises the following steps: under the protection of inert gas, carrying out a Grignard reaction on spiro [2.5] decane-6,8-diketone and an alkyl Grignard reagent or a cycloalkyl Grignard reagent, adding water for quenching after the Grignard reaction is finished, and carrying out aftertreatment purification to obtain an intermediate; and carrying out an esterification reaction on the intermediate and acryloyl chloride or methacryloyl chloride, and after the esterification reaction is finished, carrying out after-treatment purification to obtain the photoresist resin monomer. The resin monomer provided by the invention is a degradable resin monomer, and the polymer resin containing the resin monomer has better etching resistance and can improve the resolution of photoresist photoetching patterns.

The invention discloses a photoresist resin monomer synthesized from spiro[5.5]undecyl-3, 9-diketone and a synthesis method thereof, which belong to the technical field of chemical synthesis and photoetching. The structural general formula of the photoresist resin monomer is shown in the specification, in the formula, R1 is hydrogen or methyl, and R2 is saturated alkanes or cycloalkanes; the synthesis method of the spiro[5.5]undecyl-3, 9-diketone derivative comprises the following steps: carrying out a Grignard reaction on spiro[5.5]undecyl-3, 9-diketone and an alkyl Grignard reagent or a naphthenic base Grignard reagent under the protection of inert gas, adding water for quenching after the Grignard reaction is finished, and carrying out aftertreatment purification to obtain an intermediate; and carrying out an esterification reaction on the intermediate and acryloyl chloride or methacryloyl chloride, and after the esterification reaction is finished, carrying out after-treatment purification to obtain the photoresist resin monomer. The resin monomer provided by the invention is a degradable resin monomer, and the polymer resin containing the photoresist resin monomer has better etching resistance and can improve the resolution of photoresist photoetching patterns.

The invention discloses a supported catalyst, as well as a preparation method and an application of the supported catalyst in synthesis of 3,4-dihydropyrimidine-2-ketone. The supported catalyst takes granular active carbon as a carrier and is formed by absorbing copper chloride; and the loaded and absorbed copper chloride is calculated by mass percent, i.e., the ratio between the granular active carbon and the copper chloride is (85-95%):(15-5%). The supported catalyst is used for the synthetic reaction for preparing the 3,4-dihydropyrimidine-2-ketone so as to enable the synthetic reaction and purification to be completed in one step, thus not only improving the product yield, but also simplifying the operation; and therefore, the production cost is reduced. Finally, the obtained 3,4-dihydropyrimidine-2-ketone is good in color and luster as well as high in purity.

The invention relates to a preparation method for a high-temperature crosslinking agent for oil field tertiary oil recovery. The high-temperature crosslinking agent is prepared by compounding a double active group (hydroxyl methylene-CH2OH) crosslinking agent A and a crosslinking agent B according to the requirements on displacement control and profile control in different ratios, wherein the crosslinking agent B is synthesized by melamine, formaldehyde and ketone; the mass ratio of the crosslinking agent A to the crosslinking agent B of the crosslinking agent for displacement control is 5:1 to 1:1; the mass ratio of the crosslinking agent A to the crosslinking agent B of the crosslinking agent for profile control is 1:2 to 1:5; and the mass ratio of the crosslinking agent A to the crosslinking agent B of the crosslinking agent for displacement control and profile control is 1:1 to 1:3. The preparation method is scientific, is low in preparation cost and toxicity and contributes to construction and operation. Particularly, when the high-temperature crosslinking agent is applied to deep profile control, displacement control, profile control and displacement control construction in the stratum at the temperature of between 70 and 120 DEG C in the oil field tertiary oil recovery, about 26 million yuan can be created every year and the profit is 3 million yuan.

The present invention discloses an activated carbon supported phosphomolybdic tungsten heteropoly acid silver salt catalyst, and the preparation method and application in ketal synthesis. The catalyst is obtained by treating activated carbon via HNO3, adding the activated carbon into phosphomolybdic tungsten heteropoly acid solution, stirring, adding with AgNO3 solution drip by drip, standing for precipitation adsorption and then drying. The catalyst of the present invention consists of the activated carbon particles with the particle diameter of 75-800 nm loading the phosphomolybdic tungsten heteropoly acid silver salt with the weight occupying 1-50 percent, and is characterized in manageability after reaction, high activity, wide loading range and uniform activated distribution, which is suitable for the generation ketol reaction of ketone and alcohol.

The invention discloses a synthesizing method for oxidizing cobalt and manganese-based composite oxide catalyzed alcohol into aldehyde or ketone and belongs to the technical field of aldehyde or ketone synthesis. According to the method, under the action of a cobalt and manganese-based catalyst, air or oxygen is utilized as an oxidant; under the heating condition, alcohol is oxidized into corresponding aldehyde or ketone under a liquid phase. The synthesizing method disclosed by the invention has the advantage of moderate reaction conditions, reaction can be performed under the air condition,and the reaction can achieve a high-efficiency catalyzing effect of alcohol oxidization without a catalysis promoting effect of alkali, a special oxidant and / or other any organic / inorganic additive.

The invention belongs to the field of chemical synthesis, and particularly relates to a water-phase one-pot synthesis method of 3-flavonol and a 3-flavonol derivative. According to the method, 2-hydroxyacetophenone, 2-hydroxyacetophenone derivatives, benzaldehyde and benzaldehyde derivatives are used as reaction substrates, or 2-hydroxy-chalcone and hydroxy-chalcone derivatives are used as reaction substrates; water or ethanol water solution is used as a solvent; under the aerobic condition at 20 to 100 DEG C, reaction is performed to obtain the 3-flavonol and the 3-flavonol derivative. The invention provides a fire-new reaction mechanism, and develops a novel 3-flavonol synthesis method with the advantages of high efficiency, convenience, high speed and wide substrate adaptability. The invention also provides a fire-new 3-flavonol derivative synthesized by the novel method; important application values are realized in the field of medical care sanitation.

The present invention discloses a 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone synthesis process, which is characterized in that isobutyric acid is adopted as a raw material, an acylation reaction, a Friedel-Crafts reaction, and an alkaline hydrolysis reaction are performed to obtain a 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone crude product, and fine steaming is performed to obtain the 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone finished product. According to the present invention, the process is reasonable, no sulfur dioxide gas emits during the production process, the environmental pollution caused by the produced sodium chloride is low, and the product yield is high.

The invention discloses a degradable photoresist resin monomer synthesized from oxaspiro [4.5] decane diketone and a synthesis method thereof, and relates to the field of photoresist resin. The structural formula of the resin monomer is shown in the specification, R1 is saturated alkane or cycloalkane, and R2 is hydrogen or methyl. The synthesis method comprises the following steps: reacting 6-oxaspiro [4.5] decane-8, 10-diketone (I) with an alkyl Grignard reagent or a cycloalkyl Grignard reagent to obtain an intermediate (II); reacting the intermediate (II) with acryloyl chloride or methacryloyl chloride under an alkaline condition to obtain a resin monomer (III); polymer resin formed by polymerizing the resin monomer and other resin monomers has better etching resistance, is beneficial to improving the edge roughness of a developed pattern, greatly improves the resolution of a photoetching pattern, and increases the solubility of the polymer resin in a fat-soluble solvent.

The invention discloses a degradable photoresist resin monomer synthesized from pyran-3, 5-diketone and a synthesis method thereof, and relates to the field of photoresist resin monomers. The structural formula of the degradable photoresist resin monomer is shown in the specification, R1 is hydrogen or methyl, and R2 is saturated alkane or cycloalkane. The synthesis method comprises the followingsteps: carrying out Grignard reaction on 2H-pyran-3, 5 (4H, 6H)-diketone (I) and an alkyl Grignard reagent or a cycloalkyl Grignard reagent to obtain an intermediate (II); and carrying out esterification reaction on the intermediate (II) and acryloyl chloride or methacryloyl chloride to obtain a resin monomer (III). The resin monomer has better etching resistance, the difference between dissolution rates before and after exposure is increased, the improvement of the edge roughness of a developed pattern is facilitated, the resolution of a photoetching pattern is greatly improved, and the solubility of polymer resin containing the resin monomer in an ester solvent is improved.

Provided herein are methods for preparing ketone-containing organic molecules. The methods are based on novel iron / copper-mediated (“Fe / Cu-mediated”) coupling reactions. The Fe / Cu-mediated coupling reaction can be used in the preparation of complex molecules, such as halichondrins and analogs thereof. In particular, the Fe / Cu-mediated ketolization reactions described herein are useful in the preparation of intermediates en route to halichondrins.

The invention relates to a method for synthesizing photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone (1173 aryl ketone), which first uses high-purity gaseous phosgene and isobutyric acid to react to synthesize isobutyric acid Acyl chloride; in the chlorine substitution reaction, the series process is adopted, the tail gas after the first reactor is fed with chlorine is connected in series to the second reactor, and the tail gas hydrogen chloride and chlorine released by the first reaction enter the second reactor for catalytic reabsorption use. This method can improve the purity of isobutyryl chloride well, and further improve the purity and the yield of product 2-hydroxyl-2-methyl-1-phenyl-1-propyl ketone, while utilizing the catalysis of hydrogen chloride in the tail gas, The reaction speed is accelerated, the consumption of chlorine gas is reduced, and the product content is increased. The generated tail gas is recovered through harmless treatment, which solves the pollution of the tail gas to the environment.

The invention discloses a degradable photoresist resin monomer synthesized from furandione and a synthesis method thereof, and relates to the field of photoresist resin. The structural formula of theresin monomer is shown in the specification, R1 is saturated alkane or cycloalkane, and R2 is hydrogen or methyl. The synthesis method comprises the following steps: reacting furan-3, 4 (2H, 5H)-diketone (I) with an alkyl Grignard reagent or a naphthenic base Grignard reagent under the protection of inert gas, adding water for quenching after the reaction is finished, and carrying out aftertreatment and purification to obtain an intermediate (II); and 2, esterification reaction: reacting the intermediate (II) with acryloyl chloride or methacryloyl chloride under alkaline conditions, and carrying out post-treatment purification to obtain the resin monomer (III). Polymer resin formed by polymerizing the resin monomer and other resin monomers has better etching resistance, is beneficial to improving the edge roughness of a developed pattern, greatly improves the resolution of a photoetching pattern, and increases the fat solubility.

The present invention relates to a preparation method of a modified inorganic micro-nanoparticle reinforced polyether ketone ketone (PEKK) composite material. The preparation method comprises: (1) carrying out surface modification on inorganic micro-nanoparticles by using a coupling agent; and (2) directly adding the modified inorganic micro-nanoparticles at a polyether ketone ketone synthesis reaction stage. According to the present invention, the interfacial adhesion between the inorganic particles and the polyether ketone ketone polymer is improved through the coupling agent modification, and the polyether ketone ketone wraps the inorganic particles through the molecular bridge action during the molecular chain growth process, does not perform the physical blending or melt blending on the inorganic micro-nanoparticles and the polyether ketone ketone matrix, such that the inorganic particles can be well dispersed in the polyether ketone ketone matrix, the processing molding is easily achieved, and the modulus and the hardness of the polyether ketone ketone composite material are improved; and the obtained modified inorganic micro-nanoparticle reinforced polyether ketone ketone (PEKK) composite material is suitable for the fields of aerospace, industry, and medical materials.

The invention discloses methods for preparing preparing 1,4-dithiene and thiophene compounds from elemental sulfur and active internal alkyne through temperature regulation and control, and a conversion reaction of 1,4-dithiene compounds into thiophene compounds. The invention discloses the thiophene compounds synthesized through temperature regulation and a synthesis method thereof, and disclosesa process for converting the 1,4-dithiene compounds into the thiophene compounds under a high-temperature condition. Benzoyl is broken by benzoyl-substituted thiophene under high-temperature and alkaline conditions, so a green, economical, high-selectivity and high-efficiency carbon-carbon bond breaking mode is realized. According to the invention, the conversion of elemental sulfur and acetylenic ketone into the 1,4-dithiene compounds can be realized through alkali induction without metal catalysis, and the synthesis of thiophene compounds from elemental sulfur and acetylenic ketone is realized through temperature regulation and control. The synthesis method is free of metal catalysis, mild in reaction conditions, safe and simple to operate, green, economical and good in selectivity, andthe sulfur-containing compounds have good biological activity and good application prospects in the aspects of natural products and drug synthesis.

The invention provides a preparation method of methyl 4-bromoacetyl-2-methylbenzoate. The preparation method comprises the following steps: (1) dissolving 4-bromo-2-methylbenzoic acid in methanol, andperforming an esterification reaction under the catalytic action of sulfuric acid so as to produce a first intermediate compound; (2) performing a reaction between the first intermediate compound with potassium vinyl fluoroborate or vinyl boronic acid under the catalytic action of palladium so as to obtain a second intermediate compound; and (3) performing an alpha-halogenated ketone synthesis reaction on the second intermediate compound under the action of a halogenating reagent so as to obtain the methyl 4-bromoacetyl-2-methylbenzoate. The preparation method has the advantages of low raw material cost, a short route, mild reaction conditions, simple requirements for equipment and experimental conditions, large-scale amplification synthesis and a high application value.

The invention discloses a yellow polyether ketone ketone (PEKK) powder preparation method, which comprises the following steps: (a) chemically modifying the surfaces of inorganic yellow particles by using a coupling agent; (b) adding a certain proportion of the modified inorganic yellow particles in a polyether ketone ketone synthesis process, so that the modified inorganic yellow particles are inchemical bond linkage with the polyether ketone ketone; (c) smashing the yellow polyether ketone ketone composite resin obtained by the reaction, and repeatedly cleaning with ethanol and deionized water; and (d) putting the cleaned yellow polyether ketone ketone composite resin powder into a drying oven, and drying to achieve a constant weight so as to obtain the yellow polyether ketone ketone powder. According to the technical scheme, the dyeing effect is achieved through chemical synthesis instead of physical blending, the yellow polyether ketone ketone powder with the uniform color can beobtained, and the used dye is an inorganic matter, can resist high temperature, corrosion and radiation, cannot fade, and has great advantages in the aspects of use value and environmental protection.

The invention discloses a transposition method of an acetophenone isomer, and the transposition method of an acetophenone isomer comprises 2, 4-dichloroacetophenone synthesis and transposition reactions. According to the transposition method of an acetophenone isomer, a 2, 6-dichloroacetophenone isomer in crude 2, 4-dichloroacetophenone can be converted into 2, 4-dichloroacetophenone through a transposition reaction, so that the content of the 2, 6-dichloroacetophenone isomer in the crude 2, 4-dichloroacetophenone is reduced, the yield of the 2, 4-dichloroacetophenone is increased, the purification of the crude 2, 4-dichloroacetophenone is realized, the reaction is simple, and the transposition efficiency is high.