21 results about "Dimethyl acetal" patented technology

The invention provides a solid polyamine adsorption material and a preparation method thereof, and belongs to the field of adsorption materials. Comprising the following steps: carrying out selective protection reaction on polyamine and N, N-dimethylformamide dimethyl acetal in an organic solvent, so that part of active sites of the polyamine form a polyamine protecting group, and obtaining imidazoline polyamine; the preparation method comprises the following steps: carrying out a grafting reaction on imidazoline polyamine and Merrifield resin in an organic solvent, and filtering and purifying a mixed solution after the grafting reaction to obtain grafted resin spheres; and carrying out a hydrolysis reaction on the grafted resin balls and a strong alkali solution to hydrolyze and activate the polyamine protecting group, and then filtering and purifying the hydrolyzed and activated mixed solution to obtain the solid polyamine adsorption material. Compared with direct grafting of polyamine, part of active sites are protected through imidazoline of the polyamine, additional consumption of the active sites during direct grafting of the polyamine chain is avoided, and the grafting rate of the polyamine chain is high.

This invention discloses a highly efficient method for synthesizing proxalutamide intermediates, belonging to the field of pharmaceutical synthesis technology. First, dimethyl malonate and 2-chloro-5-nitropyridine are used as raw materials, condensed in the presence of potassium carbonate to generate dimethyl 2-(5-nitropyridine-2-yl)malonate. This is then reacted with tert-butyl acrylate and acid-hydrolyzed to obtain 4-(5-nitropyridine-2-yl)butyric acid. After activation with N,N'-carbonyl diimidazole, it is coupled with aminoacetaldehyde dimethyl acetal to form N-(2,2-dimethoxyethyl)-4-(5-nitropyridine-2-yl)butyramide. Then, a cyclization reaction mediated by phosphorus pentoxide and methanesulfonic acid is used to generate crude 2-(3-(5-nitropyridine-2-yl)propyl)oxazole. After purification, the nitro group is reduced by catalytic hydrogenation, and finally, it reacts with 1,5-naphthalenedisulfonic acid to form a salt, yielding the proxalutamide intermediate. This method achieves highly efficient synthesis of proxalutamide intermediates.

The application discloses a preparation method of 1,1,4,4-tetramethoxy-2-butene and application thereof, and belongs to the field of organic chemical synthesis. The method comprises the following steps: chloroacetaldehyde dimethyl acetal and triphenylphosphine are reacted to generate acetaldehyde dimethyl acetal phosphonium salt; and the acetaldehyde dimethyl acetal phosphonium salt is reacted with glyoxal monoacetal to generate 1,1,4,4-tetramethoxy-2-butene. The method is high in efficiency, environmental protection, simple in operation and friendly to the environment.

The invention belongs to the field of biomass molecule high-valued conversion, and discloses a method for high-valued conversion of a levulinic acid derivative, in particular to a method for converting the levulinic acid derivative into an organic synthesis building block, which aims at the levulinic acid derivative 4, 5-dihydro-6-methylpyridazine-3 (2H)-ketone, and converting glyoxal dimethyl acetal and 4, 5-dihydro-6-methylpyridazine-3 (2H)-ketone into an organic synthesis building block. The preparation method comprises the following steps: carrying out condensation reaction on 2, 5-dihydro-6-methylpyridazine-3 (2H)-ketone in a solvent under an alkaline condition to obtain a target acetal synthesis building block; the structural formula of the building block is shown as a formula B-1. According to the synthetic method disclosed by the invention, a synthetic route is designed, a levulinic acid derivative, namely 4, 5-dihydro-6-methylpyridazine-3 (2H)-ketone, is converted into a universal organic synthetic building block (as shown in a formula B-1), and high-value chemicals including quinoline compounds and sitroxazine can be synthesized by utilizing the synthetic building block.

The present application relates to the technical field of chemical material production, and particularly relates to a preparation method of N-(2,2-dimethoxyethyl)-1H-imidazole-1-formamide (183660-46-0); clean dichloromethane is added into a clean reaction kettle; the temperature of the reaction kettle is reduced to -5-5 DEG C, N,N'-carbonyldiimidazole is added; aminoacetaldehyde dimethyl acetal is added dropwise, and reaction is carried out for 2h; the temperature of the reaction kettle is increased, and stirring is continuously carried out at 18-25 DEG C for 12-16h, so that white suspension is obtained; normal heptane is slowly added dropwise at 18-25 DEG C, the dropwise adding time is 1-2h, stirring is continuously carried out at 18-25 DEG C for 2h, filtration is carried out under the protection of nitrogen, and the filter cake is washed once with a mixed solution of dichloromethane and normal heptane; dichloromethane and crude N-(2,2-dimethoxyethyl)-1H-imidazole-1-formamide are added, stirring is carried out at 20-25 DEG C for 30min, normal heptane is slowly added and stirred for 1h, the filter cake is collected, and drying is carried out; the fine operation of the product processing process is realized, the generation of by-products is effectively reduced, impurity wrapping and raw material residue are avoided, and the purity of the target product is improved.

The invention belongs to the field of organic synthesis, and discloses a method for preparing an indole-dipyrromethene derivative, which comprises the following steps: firstly, carrying out Ugi reaction on glyoxal dimethyl acetal, isonitrile, trifluoroacetic acid and amine to obtain an alpha-acylamino amide compound; and then under the action of an acid catalyst, carrying out [3 + 2] cyclization aromatization on the indole-dipyrromethene derivative, 4-methoxy ethyl acetoacetate and an indole derivative to obtain the indole-dipyrromethene derivative. According to the method, the indole-dipyrromethene derivative is prepared from the Ugi adduct prepared through the Ugi reaction in which glyoxal dimethyl acetal participates through [3 + 2] cyclization aromatization with ethyl 4-methoxyacetoacetate and the indole derivative, precious metal is not used in the overall reaction, the final target product can be obtained through a one-pot two-step method, and the step operation is simple. In addition, no additional ligand or additive needs to be added, and the method has the advantages of being good in reaction selectivity, high in yield, easy in product separation and the like.

The invention discloses a production process of aminoacetaldehyde dimethyl acetal, and relates to the field of organic chemical synthesis, and the production process comprises the following steps: (1) ammonification reaction: firstly mixing ammonia water and strong base to form a mixed system, adding a phase transfer catalyst into the mixed system, heating to a preset reaction temperature, slowly dropwise adding chloroacetaldehyde dimethyl acetal, and reacting for 1-2 hours at the temperature of 30-60 DEG C; according to the invention, the phase transfer catalyst is introduced as an acid-binding agent and an accelerant, the reaction temperature is controlled at 30-100 DEG C, and the whole process can be carried out at normal pressure or near normal pressure, so that the dependence of the existing process on high temperature and high pressure is thoroughly abandoned; due to the mild reaction conditions, the requirements for pressure resistance and high temperature resistance of equipment are greatly reduced, the equipment investment and the daily maintenance cost are reduced, and meanwhile, the safety risk in a high-pressure environment is avoided; on the other hand, energy consumption in the production process is remarkably reduced through the low-temperature reaction, the low-carbon chemical development trend is met, and the production cost is reduced for enterprises.

This invention relates to a method for synthesizing 1-cyclopropyl-4-oxo-7-fluoro-8-methoxy-1,4-dihydroquinoline-3-carboxylic acid, a key intermediate for numonoxacin. The method uses 2,4-difluoro-3-methoxyacetophenone as a starting material and proceeds through four steps: haloform reaction, acyl chloride formation and Maxwell's acid condensation, reaction with dimethylformamide dimethyl acetal and cyclopropylamine, and base-catalyzed cyclization and acid deprotection. This efficient method yields the target intermediate. The synthetic route of this invention utilizes readily available raw materials, mild reaction conditions, and simple operation. The multi-step reaction can be carried out in a one-pot process, achieving a total conversion rate of approximately 85% and a product purity exceeding 99.5%, making it suitable for industrial production.

The invention relates to the technical field of perfumes, in particular to an efficient condensation process in perfume synthesis, which comprises the following steps: adding styrene oxide into a methylation reagent, and reacting under the catalysis of acid; after the reaction is finished, adding an alkaline solution to adjust the pH value to 7-8, standing for layering, and taking an organic phase; and evaporating the organic phase at 50-70 DEG C to remove the solvent, and rectifying to obtain the phenylacetaldehyde dimethyl acetal. The high-efficiency condensation process in the synthesis of the perfume-phenylacetaldehyde dimethyl acetal provided by the invention has the advantages of low cost, simple process procedure, low production energy consumption, high yield, total yield of 93% or more, good product quality, purity of 98.5% or more, and wide industrial application prospect.

The invention relates to a synthesis method of 1H-pyrrolo [3, 2-B] pyridine-6-amine. Comprising the following steps: carrying out a reaction on 5-bromo-2-methyl-3-nitropyridine and N, N-dimethyl formamide dimethyl acetal to obtain (E)-2-(5-bromo-3-nitropyridine-2-yl)-N, N-dimethyl ethylene-1-amine, and carrying out a reaction on the (E)-2-(5-bromo-3-nitropyridine-2-yl)-N, N-dimethyl ethylene-1-amine and the N, N-dimethyl formamide dimethyl acetal to obtain the 5-bromo-2-methyl-3-nitropyridine. Adding the 6-bromine-4-azaindole into acetic acid, and performing reduction and cyclization reaction by using an iron-based catalyst to obtain 6-bromine-4-azaindole; and then adding into ammonia water, and reacting under a copper-based catalyst to obtain the 1H-pyrrolo [3, 2-B] pyridine-6-amine. The 1H-pyrrolo [3, 2-B] pyridine-6-amine is effectively obtained through three-step synthesis. A compound of Fe-coated PMMA-b-PDMAEMA and PE wax coated iron powder is used as an iron-based catalyst, and the ratio of the Fe-coated PMMA-b-PDMAEMA to the PE wax coated iron powder is reasonably adjusted, so that the catalytic effect of the reduction and cyclization reaction is remarkably improved and further optimized, and the conversion rate is improved, thereby realizing high yield of the product.

The invention belongs to the technical field of medicine synthesis, and provides a synthesis method of a medical intermediate 7-hydroxyfuro [3, 2-b] pyridine and an intermediate compound thereof. The preparation method comprises the following steps: taking maltol as a raw material, carrying out hydroxyl protection to obtain a compound shown in a formula II, reacting with N, N-dimethylformamide dimethyl acetal to obtain a compound shown in a formula III, reacting with alcohol under an acidic condition to obtain a compound shown in a formula IV, reacting with ammonia water to obtain a compound shown in a formula V, and carrying out dehydroxylation protection to obtain a compound shown in a formula VI. And performing dealcoholization and cyclization under an acidic condition to obtain the target compound 7-hydroxyfuro [3, 2-b] pyridine. The method has the advantages of simple synthesis steps, convenient process, simple and easily available raw materials, low cost, convenient operation method and high overall yield, and is suitable for industrial large-scale production. The intermediate compounds shown in the formula IV and the formula V and tautomers of the intermediate compounds can be used for preparing 7-chloro-6-nitrofuro [3, 2-b] pyridine as a key starting material of a JAK1 / TYK2 dual inhibitor.

The application provides a method for synthesizing an alpha, beta-unsaturated aldehyde compound by using copper as a catalyst, using an alkyne as a reaction raw material, using silane as a hydrogen source, using N, N-dimethylformamide dimethyl acetal as a formyl source, and using a carbene copper as a catalyst to efficiently synthesize the alpha, beta-unsaturated aldehyde compound. The method avoids the use of flammable and explosive and toxic synthesis gas, the raw material is cheap and easy to obtain, the reaction condition is mild, the operation is simple, the substrate has a wide application range, and excellent stereoselectivity and regioselectivity are obtained. The product alpha, beta-unsaturated aldehyde compound is an important intermediate for synthesizing complex molecules such as drugs and natural products, and the method has important significance in the fields of medicines, pesticides and fine chemicals.

The invention belongs to the field of organic matter preparation, and particularly relates to a method for purifying N, N-dimethylformamide dimethyl acetal, which comprises the following steps: amidating an amino-containing silane coupling agent by using low-molecular-weight organic acid to prepare an amide group-containing silane coupling agent; the preparation method comprises the following steps: modifying nano silicon dioxide by adopting a silane coupling agent containing an amide group to obtain modified silicon dioxide; mixing the modified silicon dioxide with a polymer, and combining with a membrane matrix to obtain a filter membrane; the method comprises the following steps: removing substances with a boiling point of below 80 DEG C in a filtrate obtained after synthesis of N, N-dimethylformamide dimethyl acetal, completing primary purification, and then continuously purifying the N, N-dimethylformamide dimethyl acetal obtained by primary purification by using a filter membrane. The method provided by the invention realizes low energy consumption, low cost and high efficiency purification of N, N-dimethylformamide dimethyl acetal.

The utility model relates to a production line for biphenyl amylene fine chemicals. An intermediate propyl cyclohexyl biphenyl formaldehyde production line, an intermediate propyl cyclohexyl biphenyl acrolein dimethyl acetal production line, a propyl cyclohexyl biphenyl propionaldehyde dimethyl acetal toluene solution production line, a propyl cyclohexyl biphenyl propionaldehyde toluene solution production line and a propyl cyclohexyl biphenyl pentene cis-trans mixture production line are adopted; the trans-propyl cyclohexyl biphenyl pentene production line and the trans-propyl cyclohexyl biphenyl pentene finished product production line are sequentially connected, and finally the trans-propyl cyclohexyl biphenyl pentene finished product is prepared through concentration of the multi-stage reaction kettle, crystallization of the crystallization kettle, filter pressing of the filter press and drying of the dryer. The production line has the functions of high efficiency and recycling, has better cost control and production efficiency, and is suitable for industrial mass production.

The invention discloses a synthesis method of 4-(diacetoxyphosphoryl)-2-methyl-2-ethyl crotonate and application of the 4-(diacetoxyphosphoryl)-2-methyl-2-ethyl crotonate, and relates to the technical field of fine chemical engineering. The synthesis method comprises the following steps: carrying out condensation reaction on halogenated acetaldehyde dimethyl acetal and ethyl propionate to form a first compound; removing methanol from the first compound to form a second compound; and carrying out a reaction on the second compound and triethyl phosphite to obtain the ethyl 4-(diacetoxyphosphoryl)-2-methyl-2-butenoate. According to the present invention, the new 4-(diacetoxyphosphoryl)-2-methyl-2-ethyl crotonate synthesis route is provided, the halogenated acetaldehyde dimethyl acetal is adopted as the starting material, the synthesis route is simple, the raw material is simple and easy to obtain, the 4-(diacetoxyphosphoryl)-2-methyl-2-ethyl crotonate yield is high, and the product yield can achieve more than 88%.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of a fenerenone intermediate 4-cyano-2-methoxybenzaldehyde. The method comprises the following steps: adding 3-methoxy-4-methylbenzonitrile into chlorobenzene, adding N, N-dimethylformamide dimethyl acetal while stirring, carrying out a heating reaction, after the reaction is finished, carrying out vacuum concentration to remove the chlorobenzene, adding an organic solvent and water, adding sodium periodate at a controlled temperature, after the heat preservation reaction is finished, carrying out centrifugal filtration to remove sodium iodate, and separating the filtrate to obtain the 3-methoxy-4-methylbenzonitrile. And concentrating and drying an organic phase, adding a saturated alkane solvent, and crystallizing to obtain the 4-cyano-2-methoxybenzaldehyde. The method has the advantages of simple synthetic route, convenience in operation, low cost, small amount of three wastes, environment friendliness, recyclable solvent and high product purity, and is more suitable for industrial mass production.

This invention belongs to the field of catalyst technology, specifically relating to the application of amino-functionalized rare earth cluster-based MOFs as catalysts in the catalytic deacetalization-Knoevenagel condensation reaction. The application method is as follows: Activated amino-functionalized rare earth cluster-based MOFs material Yb-BPDC-(NH2)2 or Dy-BPDC-(NH2)2 is placed in a reaction tube, followed by the sequential addition of the reaction substrates benzaldehyde dimethyl acetal and malononitrile. Acetonitrile is used as the solvent medium, and deionized water is added as a reaction promoter. Under continuous mechanical stirring and nitrogen protection, the reaction mixture is placed in an 80°C constant temperature oil bath for 12 hours. The amino-functionalized rare earth cluster-based MOFs material prepared by this invention exhibits excellent catalytic performance and can efficiently catalyze the deacetalization-Knoevenagel condensation reaction.

The invention belongs to the field of chemical drug synthesis, and particularly relates to a preparation method of an antibacterial drug sitafloxacin intermediate. The preparation method comprises the following steps: carrying out condensation reaction on a compound I and N, N-dimethylformamide dimethyl acetal to prepare an intermediate IV; the intermediate IV and (1R, 2S)-1-amino-2-fluorocyclopropane are subjected to a substitution reaction, and an antibacterial drug sitafloxacin intermediate compound III is prepared. The preparation method disclosed by the invention has the advantages of mild reaction conditions, short reaction time, small and single solvent dosage, high reaction conversion rate and high selectivity, and meets the requirements of industrial large-scale production.

The invention discloses a preparation method of 2-(2, 2-dimethoxyethoxy) ethylamine in the technical field of medicine production, which comprises the following steps: carrying out amino protection reaction on ethanolamine serving as a raw material, then carrying out substitution reaction with chloroacetaldehyde dimethyl acetal, removing a protecting group after the reaction, and obtaining high-purity 2-(2, 2-dimethoxyethoxy) ethylamine through a negative pressure distillation technology. The invention relates to a 2, 2-dimethoxyethoxy) ethylamine product. Through a continuous feeding method, the biggest highlight of the process is that the use of hydrazine hydrate is avoided, and the method has the advantages of safe and simple process and high yield.

The invention discloses an amino-containing polymer, a polymer film and a preparation method, the general formula of the amino-containing polymer is shown in the specification, and n is 50-200; the raw materials of the amino-containing polymer at least comprise aminoacetaldehyde dimethyl acetal and an aromatic monomer. The amino-containing polymer easy to post-modify is obtained through a one-step method by carrying out a polyhydroxyalkylation reaction on an industrial raw material aminoacetaldehyde dimethyl acetal and an aromatic monomer under an acidic condition. The raw materials required by the synthesis method can be directly purchased through industrial production, preparation and purification are not needed, and the cost is reduced; and the non-equal-metering polyhydroxyalkylation reaction is adopted, the reaction is carried out under the catalysis of acid, and the preparation condition is mild.

This invention relates to the field of organic synthesis technology and discloses a high-yield synthesis method for benzofuran-2,3-dione 3-(O-methyloxime)2-oxime. The method uses o-hydroxyacetophenone as the starting material and includes the following steps: Step 1, the starting material is refluxed with N,N-dimethylformamide dimethyl acetal in an aromatic hydrocarbon solvent to obtain an enamine ketone intermediate; Step 2, the enamine ketone intermediate is nitrosated and oxidatively cyclized using sodium nitrite and tert-butyl nitrite in a ketone solvent; Step 3, the cyclized product is reacted with methoxyamine hydrochloride in an alcohol solvent to obtain the target product. This invention avoids the use of hazardous reagents such as sodium hydride and concentrated nitric acid by constructing an enamine ketone intermediate and employing a mild two-component nitrosation system. The reaction conditions are mild, and post-processing only requires solid-liquid separation. This method has the advantages of high yield, good purity, high safety, and simple operation, making it suitable for industrial production.