43results about "Preparation by hydrogenolysis" patented technology

The invention provides a method for synthesizing a macrocyclic compound containing a conjugated diene structure through intramolecular eneyne coupling and application of the macrocyclic compound, and belongs to the technical field of organic synthesis.The method comprises the steps that a long-carbon-chain acrylamide alkyne compound and a transition metal salt catalyst are placed in an organic solvent; heating and reacting in an inert gas atmosphere to couple eneyne in molecules, and after the reaction is finished, carrying out post-treatment on a reaction solution to obtain a macrocyclic compound containing a conjugated diene structure; according to the method, iridium salt is used for catalyzing intramolecular eneyne coupling to synthesize the macrocyclic compound containing the conjugated diene structure, the synthesis efficiency is high, the method is environmentally friendly, the production environmental protection pressure is small, the method is wide in substrate application range, the method can be used for synthesizing 12-26-membered all-carbon and / or ether macrocyclic compound containing the conjugated diene structure, the atom economy is good, and the method is suitable for industrial production. The reaction yield is high, and the method has a wide application prospect in the field of organic synthesis.

To provide methods for producing trifluoromethyl ketone and pentafluoroethyl ketone in economical, safe and industrial manners.SOLUTION: An ester compound represented by the general formula (1) is supplied and mixed with a base and trifluoromethane or pentafluoroethane in the presence of organic solvent by using a micro mixer and a micro reactor, and the reaction of them results in a trifluoromethyl ketone or pentafluoroethyl ketone represented by the general formula (3). [R1 is a naphthyl-1-yl group or the like; R2 is a methyl group or an ethyl group; Rf is a trifluoromethyl group or pentafluoroethyl group].SELECTED DRAWING: None

A method for producing bisphenol A that can efficiently remove coloring components derived from a polycarbonate resin to enable production of bisphenol A having good color tone is provided. In the method of the present invention for producing bisphenol A, a solution H1 or a solution H2 is obtained from a crude solution A obtained by degrading a polycarbonate resin (PC) and distilling off a solvent in step A and part of a mother liquor D obtained in step D of step B to step E to produce bisphenol A (BPA) by dehydration condensation of acetone and phenol, and the solution H1 or the solution H2 obtained is supplied to the step B or the step C. The solution H1 is a solution containing BPA obtained by degrading BPA contained in the crude solution A and the mother liquor D into phenol and isopropenylphenol and then rebonding phenol and isopropenylphenol, and the solution H2 is a solution containing phenol obtained by degrading BPA contained in the crude solution A and the mother liquor D into phenol and acetone.

The invention relates to the technical field of compound synthesis, in particular to a method for directly reducing carboxylic acid into aldehyde. The preparation method comprises the following steps: mixing triphenylphosphine, dichloromethane, carboxylic acid and N-chlorosuccinimide, and reacting to obtain a reactant; mixing with pinacol borane and 4-dimethyl pyridine, and continuously reacting to obtain a continuous reactant; and separating and purifying to obtain aldehyde. The synthesis of the substrate carboxylic acid provided by the invention and the rapid deoxidation of the carboxylic acid are carried out to obtain an aldehyde product, especially the following compounds 2aa, 2ab, 2ae, 2bc, 2be, 2bf, 2bg, 2bh, 2bi, 2bj, 2bk and 2bl have catalytic hydrolysis effects on hypophosphamide; the compound 2bl has a particularly excellent effect on hydrolysis of hypophosphamide.

The invention relates to the technical field of photoelectric materials, in particular to a novel process of ultra-pure TFT (thin film transistor) negative monomer liquid crystal for a large-size panel, which comprises the following steps: S1.1, preparing 4-chlorophenyl cyclohexane formaldehyde from 4-(4-chlorophenyl) cyclohexanecarboxylic acid; S1.2, performing protection treatment on the 4-chlorophenyl cyclohexane formaldehyde, and preparing 4-alkyl biphenyl cyclohexane formaldehyde from the 4-chlorophenyl cyclohexane formaldehyde; s1.3, preparing a negative monomer liquid crystal; according to the preparation method, 4-(4-chlorphenyl) cyclohexanecarboxylic acid is directly reduced into 4-chlorphenyl cyclohexane formaldehyde by using a loaded reducing agent, and oxidation after excessive reduction is not needed, so that two-step reaction in a traditional process is reduced into one step, and the preparation process is simpler and more convenient.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of octadecanedioic acid mono-tert-butyl ester. The method specifically comprises the following steps: reacting dodecanedioic acid, dichloromethane and DMF (Dimethyl Formamide), controlling the temperature, dropwise adding an acylation reagent, and performing reduced pressure concentration after reaction to obtain a compound 1; reacting the compound 1, dimethylbenzene, palladium-carbon and organic alkali, carrying out nitrogen displacement, introducing hydrogen at a controlled temperature, carrying out nitrogen displacement after the reaction, and filtering and concentrating to obtain a compound 2; adding tert-butyl acrylate into an acetic acid aqueous solution, dropwise adding the compound 2, reacting, adjusting the pH value, extracting, filtering and concentrating to obtain a compound 3; adding the compound 3 into dichloromethane, controlling the temperature, adding aluminum trichloride, dropwise adding a reducing agent, reacting, filtering, adjusting the pH value, separating liquid, concentrating and recrystallizing to obtain di-tert-butyl octadecanedioate; and reacting the di-tert-butyl octadecanedioate, lithium hydroxide and tert-butyl alcohol, filtering, adjusting the pH value, extracting, concentrating and recrystallizing to obtain the mono-tert-butyl octadecanedioate. The method is low in production cost and high in safety.

The invention relates to the technical field of organic synthesis, particularly discloses a preparation method of superior tiderone and an intermediate of superior tiderone, and provides a gram-scale superior tiderone synthesis route which is simple, efficient, simple in reaction operation and easy to amplify. The longest linear step 12 of the route is the shortest synthetic route in the current molecular synthesis report. In addition, initial raw materials and synthetic reagents are cheap and easy to obtain, and the cost of synthetic materials is greatly reduced. According to the route, a highly-converged synthesis strategy is adopted, and fragment assembly is more flexible. Therefore, on the basis of the route, a plurality of fragments are subjected to derivatization modification and assembly, and a structure based on the optitiderone can be efficiently obtained, so that a solid material foundation is laid for finding anti-tumor active molecules.

To provide a use for novel triaryl borane type catalyst compounds which can be applied for the partial reduction of an ester or lactone to a silyl acetal.SOLUTION: The present invention relates to a use of compounds of general formula (Ia) as catalysts for partial reduction of a carbonyl group in an ester substrate or lactone substrate, wherein the substrate contains one or more functional group(s) independently selected from the group consisting of non-carbonyl-conjugated olefinic bonds, non-carbonyl-conjugated acetylenic bonds, ether, amide, and halogen groups.SELECTED DRAWING: None

The invention relates to the technical field of organic synthesis, in particular to a preparation method of cyclopropyl formaldehyde, which comprises the following steps: by taking methyl cyclopropyl formate as a raw material, red aluminum as a reducing agent and toluene as a solvent, carrying out heat preservation reaction under the protection of nitrogen and controlling the reaction temperature to be not more than-78 DEG C; after the reaction is finished, firstly carrying out quenching reaction by using absolute ethyl alcohol, then adding a saturated ammonium chloride solution for further quenching reaction, then adjusting the pH value to be acidic, layering, collecting a water phase, extracting, combining the collected organic phase, drying, filtering, and then carrying out distillation treatment on the material liquid, so as to obtain the product. And rectifying the material liquid without the extracting agent to obtain a cyclopropyl formaldehyde product. The process method can reduce the cost, is suitable for industrial production, and greatly improves the yield and purity of the cyclopropyl formaldehyde product.

The invention discloses a novel perylene diimide coordination polymer as well as a preparation method and application thereof, and belongs to the technical field of coordination polymers. The chemical formula of the novel perylene diimide coordination polymer provided by the invention is C44H20Cl4N4O8Zn, and the novel perylene diimide coordination polymer has good thermal stability and chemical stability, can stably exist in a 100 DEG C aqueous solution, an acetonitrile solution or an N, N-dimethylformamide solution for 24 hours, and can resist the heat up to 300 DEG C in a nitrogen atmosphere. Besides, the novel perylene diimide coordination polymer provided by the invention has the characteristics of high conversion rate and high chemical stability as a photocatalyst, has extremely high photocatalytic activity on a reaction of converting aryl acetic acid into an aryl formaldehyde derivative, and is low in dosage.

Disclosed are a fluorenylaminoketone photoinitiator, a preparation method thereof, and a UV photocurable composition containing same. The photoinitiator comprises a compound having a structure as shown in general formula (I) or a derivative compound thereof. The fluorenylaminoketone photoinitiator provided in the present invention may effectively improve the solubility of traditional photoinitiators and reduce the use of micromolecular active diluents, and also has high sensitivity and good effect of deep-layer curing. It has very good promotion effect on popularization and application of photocurable compositions, particularly colored ink systems, in the field of photocuring. The UV photocurable composition containing a fluorenylaminoketone photoinitiator of the present invention has advantages of high sensitivity, no residue after development, good pattern integrity, and no or little odor of coating layers after curing, as well as excellent yellowing resistance.

The invention provides a synthetic method of an Advantame intermediate 3-(3-hydroxy-4-methoxyphenyl)-1-propionaldehyde, which comprises the following steps: step 1, carrying out Wittig reaction on isovanillin and cyano methylene triphenylphosphine to generate 3-(3-hydroxy-4-methoxyphenyl) acrylonitrile; step 2, carrying out hydrogenation reaction on the 3-(3-hydroxy-4-methoxyphenyl) acrylonitrile under the catalysis of Pd / C, so as to obtain 3-(3-hydroxy-4-methoxyphenyl)-1-propionitrile; and step 3, reducing the 3-(3-hydroxy-4-methoxyphenyl)-1-propionitrile by using diisobutylaluminium hydride, so as to obtain the 3-(3-hydroxy-4-methoxyphenyl)-1-propionaldehyde. The synthesis method is mild in reaction condition, high in overall yield and high in product purity.

To provide a method for producing acetaldehyde and ethanol by reacting carbon dioxide and methane in a gas phase by applying a voltage to a catalyst, which is improved in at least one of an STY ratio (acetaldehyde STY / carbon monoxide STY) between acetaldehyde as an objective substance and carbon monoxide as an intermediate substance and an STY ratio (ethanol STY / carbon monoxide STY) between ethanol as an objective substance and carbon monoxide as an intermediate substance.SOLUTION: Provided is a method for producing acetaldehyde and ethanol by reacting a carbon dioxide and methane in a gas phase in the presence of a catalyst at a reaction temperature 80 to 400°C, while an electric current is applied to the catalyst in which rhodium (Rh) and an oxide of at least one element selected from the group consisting of titanium (Ti), vanadium (V), molybdenum (Mo), tungsten (W) and manganese (Mn) are supported on semiconductor carriers having a band gap of 3.3 to 6.0 eV.SELECTED DRAWING: Figure 2

A method of preparing a triterpenoid compound of formula (I):including a step of converting a compound of formula (II) into the compound of formula (I),wherein R1 and R2 independently represent hydrogen or a protecting group selected from the group consisting of C1-C8 alkyl, allyl, C2-C8 alkenyl, C2-C8 alkynyl, (C6-C12)aryl(C1-C8)alkyl, tri(C1-C8)alkylsilyl, di(C1-C8)alkyl(C6-C12)arylsilyl, di(C6-C12)aryl(C1-C8)alkylsilyl ,tri(C6-C12)arylsilyl, —C(O)R7, and —C(O)OR8, and each of which is substituted with from 0 to 4 substituents independently selected from the group consisting of hydroxy, cyano, halo, halo(C1-C6)alkyl, halo(C1-C6)alkyloxy, (C1-C6)alkylthio, C1-C6 alkyl, C2-C6 alkenyl, C2-C6 alkynyl, C3-C7 cycloalkyl and C1-C6 alkoxy, wherein R7 and R8 are independently C1-C8 alkyl or C6-C12 aryl.

The present invention provides a method for preparing pure isopropanol from carbon dioxide, and the synthesis route is as follows: 1) using a membrane electrode assembly reactor and a nickel single atom-nitrogen doped activated carbon material to electrocatalytically reduce carbon dioxide to pure carbon monoxide; 2) using a solid electrolyte electrolytic cell and a copper gel material to electrocatalytically reduce carbon monoxide to pure acetic acid; 3) using a cerium oxide material to catalyze the acetic acid ketolysis reaction at 300°C and normal pressure to obtain acetone and carbon dioxide, wherein the carbon dioxide can be recycled to step 1 for recycling; 4) using a bipolar membrane membrane electrode assembly reactor and a lattice stretched ruthenium metal nanocatalyst to electrocatalytically reduce pure acetone to pure isopropanol liquid. The present invention proposes a potential solution for the highly selective, mild and green preparation of carbon dioxide to isopropanol by integrating the two-step electrolysis of carbon dioxide, acetic acid ketolysis and acetone electroreduction reactions.

Provided is a method which is for producing bisphenol A and by which a colored component derived from a polycarbonate resin can be efficiently removed, and bisphenol A having a favorable color tone can be produced.　A method for producing bisphenol A according to the present invention involves: obtaining a solution H1 or a solution H2 from a crude solution A, which is obtained by decomposing a polycarbonate resin (PC) and distilling a solvent in step A, and from part of a mother liquid D, which is obtained in step D among steps B to E for producing bisphenol A (BPA) through the dehydration condensation of acetone and phenol; and supplying the obtained solution H1 or solution H2 to step B or step C. The solution H1 is a solution that contains BPA obtained by decomposing the BPA contained in the crude solution A and the mother liquid D into phenol and isopropenylphenol and then re-bonding the phenol and the isopropenylphenol, and the solution H2 is a solution that contains phenol obtained by decomposing BPA contained in the crude solution A and the mother liquid D into phenol and acetone.

Provided: A method for manufacturing bisphenol A capable of efficiently removing coloring components derived from polycarbonate resin and producing bisphenol A with good color tone. In the bisphenol A manufacturing method of the present invention, a crude solution A obtained by decomposing polycarbonate resin (PC) in step A and removing the solvent by distillation, and a portion of a mother liquor D obtained in step D of steps B to E (where bisphenol A (BPA) is manufactured by dehydration condensation of acetone and phenol), are used to obtain solution H1 or solution H2. Solution H1 or solution H2 is supplied to step B or step C. Solution H1 is a solution containing BPA obtained by decomposing BPA contained in crude solution A and mother liquor D into phenol and isopropenylphenol, and then recombinating the phenol and isopropenylphenol. Solution H2 is a solution containing phenol obtained by decomposing BPA contained in crude solution A and mother liquor D into phenol and acetone.

The present disclosure relates to a method that includes processing, in a hydrodeoxygenation (HDO) reactor, at least one of a VFA-derived ketone and / or a co-processing stream to produce a composition that is at least partially bioderived, as determined by ASTM-D6866.

The application discloses a bimetallic catalyst for preparing o-phthalaldehyde by dimethyl phthalate hydrogenation and a preparation method thereof, and belongs to the field of catalyst preparation and application. The Ni-Fe / Al2O3-ZrO2 catalyst loaded with nickel and iron bimetal is prepared by taking alumina and zirconium dioxide as carriers, wherein n(Ni):n(Fe):n(Al):n(Zr) = 0.1:0.05:2:1. The Ni-Fe / Al2O3-ZrO2 catalyst is prepared by first preparing a Ni-Fe / Al2O3-ZrO2 catalyst precursor and then carrying out a reduction reaction in a hydrogen atmosphere. The Ni-Fe / Al2O3-ZrO2 catalyst of the application will not be deactivated due to carbon deposition and metal sintering in the high-temperature hydrogenation process, prolongs the service life of the catalyst, promotes the reaction of preparing o-phthalaldehyde by dimethyl phthalate hydrogenation, and has great competitive advantages.

The present invention generally relates to the production of vanillin and related compounds (such as aromatic carboxylic acids, quinones, etc.) involving the oxidative cleavage of aromatic compounds (such as lignin, lignols, cinnamic acid and its derivatives, etc.) under mild reaction conditions. More specifically, the present invention provides processes for the production of vanillin involving the oxidative cleavage of an aromatic compound, such as lignin or ferulic acid, using a peroxide based oxidant, such as hydrogen peroxide, in the presence of a suitable catalysis, such as vanadium oxide.

The present disclosure relates to a method for preparing a compound as an intermediate for synthesizing the drug posaconazole and the intermediate compounds prepared thereby. The method for preparing a compound of Formula I provided in the present disclosure comprises: firstly reacting 4-(2,4-difluorophenyl)pent-4-enoate or its reduction product 4-(2,4-difluorophenyl)pent-4-enal as a starting material with formaldehyde or paraformaldehyde in the presence of a chiral catalyst, and then subjecting the reaction product to a characteristic oxidation, an esterification, a halogenation and cyclization reaction, finally a hydrolysis and an acid treatment. The preparation method of the present disclosure has advantages such as mild reaction conditions, simple reaction process, and high overall yield and high purity of target products, and thus is suitable for industrial production.

This invention relates to the field of electrochemistry, specifically disclosing a method for the selective electrooxidation of polyhydroxy compounds. More specifically, it involves the selective electrooxidation of compound (Ⅰ) to obtain compound (Ⅱ). This invention reduces the large number of byproducts caused by the simultaneous oxidation of multiple pairs of hydroxyl groups in traditional oxidation methods. By selectively electrooxidizing to obtain compound (Ⅱ), and then reducing compound (Ⅱ) to obtain compound (Ⅲ), for example, selectively electrooxidizing hydroxycitronellol (3,7-dimethyl-1,7-octanediol, compound 1a) to obtain (7-hydroxy-3,7-dimethyloctanoic acid, compound 2b), and then reducing it with compound 1b to obtain compound 1c. Compound 1c is hydroxycitronellol (CAS: 107-75-5), which has a strong floral fragrance. By changing the number of carbon atoms in hydroxycitronellol without changing the functional groups, a series of small molecule compounds with different fragrances can be produced efficiently and with low pollution.

The invention provides a preparation method of nabumetone, which comprises the following steps: S1, sequentially adding 6-methoxy-2-naphthol and ethyl acetate into an organic solvent under the condition of high-pressure microjet, adjusting the pH value to 5.5-6.5, adding a catalyst, reacting under the condition of a low-frequency ultrasonic field, and filtering after the reaction is finished to obtain an intermediate product; and S2, adding the intermediate product into an organic solvent, adding the catalyst in S1, introducing hydrogen for reaction, and after the reaction is finished, filtering, concentrating under reduced pressure and crystallizing to obtain nabumetone. The high-pressure microjet method is utilized to accurately control the dosage of the reaction raw materials, increase the contact area of the reaction raw materials, reduce the reaction time and improve the reaction rate, the high-pressure microjet combined with the low-frequency ultrasonic field can remarkably reduce side reactions and improve the purity of the target product, and in addition, the reaction efficiency and the reaction selectivity can be improved; the total yield of the product is improved, and the application prospect is good.

The invention belongs to the technical field of ethanol synthesis, and discloses a gas-liquid combined two-step method acetic acid hydrogenation device and process. The device comprises a heating mixer, a reactor, a gas-liquid separator, a liquid phase hydrogenation reaction kettle, a separator and a rectifying tower which are connected in sequence. The process comprises three working sections of acetic acid hydrogenation, acetaldehyde and acetic ether hydrogenation and crude product purification. Acetic acid is hydrogenated under the action of a catalyst to prepare acetaldehyde and acetic ether, in the acetaldehyde and acetic ether hydrogenation section, a reaction mixture in the acetic acid hydrogenation section is directly hydrogenated to prepare ethanol, hydrogen-rich tail gas and fresh hydrogen are mixed and enter the acetic acid hydrogenation section to serve as reaction gas, crude ethanol is rectified and purified, and high-purity ethanol is obtained. According to the invention, continuous production is realized, the hydrogen is subjected to deep reaction, the raw materials have higher conversion rate and yield, and the operation continuity and stability are very high. The corrosion of direct hydrogenation of acetic acid to equipment is reduced, and the defects of high energy consumption and huge equipment scale caused by an ethanol system are avoided.

To provide a novel catalyst for hydrogen combustion reaction.SOLUTION: A catalyst for hydrogen combustion reaction comprises at least one kind selected from the group consisting of silver carbonate (Ag2CO3), silver acetate (CH3COOAg), and silver oxide (Ag2O).SELECTED DRAWING: Figure 1

The application belongs to the technical field of organic synthesis and particularly relates to a preparation method of monotert-butyl octadecanedioate. Specifically, dodecanedioic acid, dichloromethane and DMF are reacted, temperature is controlled, an acylation reagent is added dropwise, compound 1 is obtained after reaction and concentration under reduced pressure; compound 1, dimethylbenzene, palladium charcoal and an organic base are reacted, nitrogen is replaced, hydrogen is introduced under temperature control, nitrogen is replaced after reaction, filtration and concentration are performed, and compound 2 is obtained; tert-butyl acrylate is added into an acetic acid aqueous solution, compound 2 is added dropwise, reaction is performed, pH is adjusted, extraction is performed, filtration and concentration are performed, and compound 3 is obtained; compound 3 is added into dichloromethane, temperature is controlled, aluminum chloride is added, a reducing agent is added dropwise, reaction is performed, filtration is performed, pH is adjusted, liquid separation is performed, concentration and recrystallization are performed, and di-tert-butyl octadecanedioate is obtained; di-tert-butyl octadecanedioate, lithium hydroxide and tert-butyl alcohol are reacted, filtration is performed, pH is adjusted, extraction is performed, concentration and recrystallization are performed, and monotert-butyl octadecanedioate is obtained. The method has low production cost and high safety.

The present disclosure relates to a method for preparing a compound as an intermediate for synthesizing the drug posaconazole and the intermediate compounds prepared thereby. The method for preparing a compound of Formula I provided in the present disclosure comprises: firstly reacting 4-(2,4-difluorophenyl) pent-4-enoate or its reduction product 4-(2,4-difluorophenyl) pent-4-enal as a starting material with formaldehyde or paraformaldehyde in the presence of a chiral catalyst, and then subjecting the reaction product to a characteristic oxidation, an esterification, a halogenation and cyclization reaction, finally a hydrolysis and an acid treatment. The preparation method of the present disclosure has advantages such as mild reaction conditions, simple reaction process, and high overall yield and high purity of target products, and thus is suitable for industrial production.

Provided herein is a method for preparing a biowax, comprising: (i) providing a raw material containing one or more fatty acids having 12 to 22 carbon atoms; and (ii)(a) a layered double oxide; (b) a binder; subjecting said feedstock to a ketonization reaction catalyzed by a composite catalyst material comprising: A method is disclosed that includes:

The invention belongs to the technical field of catalytic conversion of bulk chemicals, and particularly relates to a method for preparing acetaldehyde and co-producing ethanol from synthesis gas and a preparation method of a catalyst thereof. The method for preparing acetaldehyde and co-producing ethanol from synthesis gas provided by the invention comprises the following steps: (1) a first stage: under the action of a CuZnAl catalyst and a molecular sieve, carrying out hydrogenation on the synthesis gas to generate methanol, dehydrating the methanol to generate dimethyl ether, and carrying out carbonylation on the dimethyl ether to synthesize methyl acetate; and (2) a second stage: under the action of the Mn-based catalyst, hydrogenating methyl acetate to prepare acetaldehyde and co-produce ethanol. The catalyst adopted by the method is low in cost, simple in synthesis, high in acetaldehyde selectivity, simple in technological process, high in safety coefficient and less in three wastes.