91 results about "Enone" patented technology

The invention belongs to the technical field of organic matter preparation, and particularly relates to a preparation method of 2-pentylcyclopentyl-2-ketene. According to the method, methanol is used as a solvent, sulfonic acid type resin doped with lewis acid is used as a catalyst to catalyze the isomerization reaction of 2-pentylidene cyclopentanone, the catalyst and the methanol solvent can jointly promote the isomerization reaction of 2-pentylidene cyclopentanone, and the catalytic efficiency is high, so that the reaction yield is remarkably increased, and the catalyst cost is reduced; in addition, a fixed bed reactor continuous production mode is adopted, waste salt is prevented from being generated when the acid catalyst is quenched by processes such as HCl / HBr / p-toluenesulfonic acid, and methanol is used as a solvent, so that the byproduct dimethyl ether is simply separated from water and the solvent methanol. In addition, when the sulfonic acid type resin doped with the lewis acid is used for catalyzing the isomerization reaction of 2-pentylidene cyclopentanone, the stability is high, and the service life is long.

The invention belongs to the technical field of isomer separation, and provides a separation method of megastigmatrienone isomers. The method comprises the following steps: mixing megastigmatrienone with methanol to obtain a mixed solution, and filtering the mixed solution by adopting an organic phase filter membrane; and then separating the filtered mixed solution by adopting a reversed-phase preparative chromatography to obtain the isomer of megastigmatrienone. According to the separation method, different isomers of megastigmatrienone can be obtained through efficient separation, and the separation method is environmentally friendly, easy to operate and easy to implement.

An object of the present disclosure is to provide a crystalline form of 3-(15-methoxypentadecyl)-2, 4, 4-trimethylcyclohex-2-en-1-one, the crystalline form having excellent stability and being preferable in terms of production. The present disclosure provides a crystalline form having characteristic peaks at diffraction angles) (2θ+0.2° of 7.0°, 14.0°, 17.5°, 19.5°, 21.0°, 23.7°, and 24.8° in a powder X-ray diffraction spectrum (CuKα).

The invention provides a preparation method of polar polyolefin, and belongs to the technical field of polyolefin. The preparation method comprises the following steps: in an inert atmosphere, under the action of a catalyst and a cocatalyst, copolymerizing C2-C6 olefin and an alkylated polar monomer in an organic solvent to prepare polar polyolefin, wherein the alkylated polar monomer is prepared by the following steps: dissolving an alkylating reagent in an organic solvent, adding a polar monomer, and mixing and stirring to obtain the alkylated polar monomer; the polar monomer comprises at least one of halogenated alpha-olefin, alpha-olefine acid, alpha-enol, alpha-olefine aldehyde, alpha-olefine ester and alpha-olefine ketone. The polar monomer is pre-protected by adding the alkylating reagent, so that effective copolymerization of C2-C6 olefin and the polar monomer is realized, and the performance of polyolefin is favorably improved.

The invention relates to an industrial preparation method of an intermediate 5alpha-androstane-2-ene-17 ketone, the intermediate is a rocuronium bromide intermediate, and the method comprises the following steps: taking epiandrosterone as a starting material, and reacting with paratoluensulfonyl chloride to obtain a compound I; and carrying out elimination reaction on the compound I in organic alkali or a DBU catalyst to obtain the compound 5 alpha-androstane-2-ene-17 ketone. The method is good in elimination reaction selectivity, high in yield, good in quality, low in cost, mild in reaction condition, short in production period, recyclable in reaction solvent and green and environment-friendly in production process, and a single impurity of the product is less than 0.3%.

The invention discloses a preparation method of galanthamine and an intermediate thereof, and belongs to the technical field of organic chemical synthesis. The chemical structural formulas of the intermediates for synthesis of galanthamine are as shown in formulas (I)-(IV). According to the invention, 2-cyclohexenone, acrylic ester, 3-hydroxy-2-halo-4-methoxybenzaldehyde and the like are used as starting raw materials, and the intermediate required for preparing the galanthamine is synthesized in sequence through a plurality of reactions such as Sentian-Bellies-Hilmann reaction, Corey-Barksh-Chai-field reaction, Mitsunobu reaction and the like; and then the galanthamine is synthesized by using the intermediates. The synthesis method is low in raw material and reagent price, low in production cost, short in synthesis route, easy and convenient to operate, high in yield and suitable for large-scale production, and the problems that an existing galanthamine synthesis process is complex, high in cost, low in yield and the like are solved.

The invention discloses application of a trienone compound in anti-tumor drugs, and belongs to the technical field of application of anti-tumor drugs. Through MTT cell viability experiments, cancer cells are treated by the trienone compounds with different concentrations, a good cell viability inhibition effect is found, and the inhibition effect of the four trienone compounds is superior to that of a positive drug cis-platinum. The trienone compound provided by the invention can be used for preparing or developing an anti-tumor drug, can contain a carrier and an auxiliary agent, can be prepared into a tablet, a particle, a capsule, an oral liquid or an injection form, and has a good practical application prospect.

The application provides a reverse Markovnikov hydroamination reaction of trifluoromethyl enone under catalyst-free and base-free conditions, uses a sulfonhydrazide compound with good functional group tolerance as a nitrogen source, realizes the introduction of a nitrogen-containing functional group in a green and environment-friendly manner, and synthesizes a series of alpha-sulfonhydrazine-alpha-hexafluoroisopropyl-substituted carbonyl compounds. The method has the characteristics of no transition metal participation, mild conditions, wide substrate universality and the like.

The invention discloses a desaturase TgDH. The desaturase TgDH has an amino acid sequence as shown in SEQ ID No. 2 or SEQ ID No. 3. The desaturase TgDH is used as a biocatalyst, and the chiral ketene compound can be synthesized with high yield and high stereoselectivity. A catalytic asymmetric technical route of the enzyme is mild in reaction condition, environment-friendly and high in selectivity, the catalyst is cheap and easy to obtain, separation and purification are simple and convenient, the optical purity is greater than 99% ee, and the actual separation yield (77%) is relatively high. The invention discloses a method for asymmetrically synthesizing a chiral 4-substituted cyclohexenone compound, which takes a 4-substituted cyclohexanone compound as a substrate, takes desaturase TgDH or whole cells containing the desaturase TgDH as a catalyst and reacts in a solvent to obtain the chiral 4-substituted cyclohexenone compound.

The application belongs to the technical field of chemical synthesis, and particularly relates to a synthesis method of 2-aryl-2-cyclohexanedione enol ester compounds. The method uses a transition metal complex as a catalyst, and uses a phenyl boronic acid compound and an iodine onium compound as raw materials, first synthesizes a 3-hydroxy-2-aryl-2-cyclohexenone compound, and then synthesizes the 2-aryl-2-cyclohexanedione enol ester compound through acylation. The reaction condition is mild, no additional additives (such as alkali-sodium acetate, expensive silver salt-silver acetate, etc.) need to be added, the C-C bond can be efficiently and quickly constructed, the 2-aryl-2-cyclohexanedione cyclization derivative is obtained, the reaction operation is simple, the reaction time is short, the method has high efficiency and high safety, the substrate range is wide, the functional group tolerance is good, the method conforms to the concept of green chemistry and high atomic economy, and is very suitable for large-scale industrial production.

The invention relates to the technical field of microorganisms, in particular to a method for synthesizing 7 alpha, 11 alpha, 22-trihydroxy-23, 24-dinorchol-4-ene-3-ketone by microorganisms. The invention provides gibberella fujikuroi GBC-40272-A which is preserved in the general microbiological center of the China Committee for Culture Collection of Microorganisms, and the preservation number of the gibberella fujikuroi GBC-40272-A is CGMCC (China General Microbiological Culture Collection Center) No.40586. The strain can efficiently convert 4-HBC to synthesize 7 alpha, 11 alpha-dihydroxy-4-HBC, and has the advantages of high conversion rate, high selectivity and high product yield. The method for synthesizing the 7alpha, 11alpha-dihydroxy-4-HBC by utilizing the microorganisms, provided by the invention, is high in conversion rate and short in conversion period, provides an important precursor compound for synthesis of a steroid drug, also provides a new method for synthesis of the steroid drug, and is relatively good in application prospect.

The invention discloses a method for synthesizing 4-hydroxycyclopentyl-2-ketene by catalyzing rearrangement of furfuryl alcohol with a copper-based bimetallic oxide, which is characterized in that under the action of a copper-based composite metal oxide catalyst, furfuryl alcohol is subjected to one-step conversion in a stainless steel autoclave to generate a target product 4-hydroxycyclopentyl-2-ketene, wherein the heterogeneous catalyst is a CuX type composite bimetallic oxide, X is selected from one of La, Bi, Fe, Ce, Ga and Cr, and the theoretical atomic number ratio of Cu to X is (1-5): 1. And a novel, simple and efficient synthesis method is provided for the preparation of the renewable 4-hydroxycyclopentyl-2-ketene.

The application relates to the technical field of chemical synthesis, and particularly discloses a method for constructing cycloalkanol by nickel-catalyzed asymmetric hydrogenation of tri-substituted enone, and a chiral alcohol prepared by the method. The method uses alpha, beta-unsaturated ketone with different molecular structures as a substrate to construct chiral alcohol with double chiral centers, hydrogen is added to reduce the enyl group first, and then hydrogen is added to reduce the carbonyl group. In the case that the hydrogen on the carbon in the conjugated ring is replaced by different substituents, good reduction effect can be obtained. The catalyst has simple preparation mode and stable performance, and good chiral selection effect and conversion rate can still be obtained under the condition of high substrate / catalyst.

The invention discloses a method for separating and preparing megastigmatrienone isomers, and belongs to the technical field of isomer separation and preparation. The technical problem to be solved is that in the prior art, mg-level separation preparation of a megastigmatrienone single-configuration isomer cannot be rapidly realized. The key point of the technical scheme is as follows: the method comprises the following steps: (1) mixing megastigmatrienone with methanol to obtain a mixed solution; (2) separating the mixed solution by adopting a reversed-phase preparative chromatography to obtain an isomer of megastigmatrienone; wherein the chromatographic conditions in the reversed-phase preparative chromatography in the step (2) are as follows: a chromatographic column is a reversed-phase semi-preparative chromatographic column, the sample size is 100-800 [mu] L, the flow velocity is 0.1-0.8 mL / min, the detection wavelength is 308 nm, an eluent is methanol-THF-H2O in a ratio of 37.5: 7.5: 55, and isocratic elution is performed.

This invention discloses a high-adhesion optical adhesive for extreme conditions, its preparation method, and its application, belonging to the field of optical adhesive technology. It comprises the following components in parts by weight: 20-30 parts of 2-methyl-6-methylene-1,7-octadien-3-one, 15-25 parts of 1,4-butanediol dimethacrylate, 15-25 parts of tetraethylene glycol dimethacrylate, 5-10 parts of α-methacrylic acid, 5-10 parts of hydroxyethyl methacrylate, 2-5 parts of vinyltriethoxysilane, 0.1-0.5 parts of 1-hydroxycyclohexylphenyl ketone, 0.1-0.5 parts of 2-hydroxy-2-methyl-1-phenyl-1-propanone, and 0.3-0.5 parts of 1-[9-ethyl-6-(2-methylbenzoyl)-9H-carbazole-3-yl]acetone-1-(O-acetyloxime). The optical adhesive of the present invention has excellent bonding performance and can prevent the bonded components from debonding and causing cohesive failure at the bonding joint in humid, steamy, or chemical solvent environments.

A first aspect of the invention relates to a mixture comprising 2,4- toluene diamine and 2,6-toluene diamine and comprising less than 10 weight-ppm of an amino methyl cyclohexenone compound of formula (I) based on the total weight of the mixture being 100 weight-%. In a second aspect, the invention is directed to a method for controlling a hydrogenation process for preparing toluene diamine (TDA) from dinitrotoluene (DNT), said TDA having a boiling temperature range BTRTDA with a lower boiling temperature limit value TTDA(L) and an upper boiling temperature limit value TTDA(U). A third aspect relates to a mixture comprising at least 2,4- toluene diamine and 2,6-toluene diamine obtained or obtainable from the method according to the second aspect. A fourth aspect of the invention is directed to a use of the mixture according to the first aspect of the invention or of the mixture of the third aspect of the invention for the preparation of toluene diisocyanate (TDI). In a fifth aspect, the invention relates to a process for preparing toluene diisocyanate (TDI) comprising: (I) Providing a mixture according to the first aspect of the invention or of the mixture of the third aspect of the invention; and (II) Phosgenation of the mixture provided in (I), thereby obtaining TDI.

The present application relates to a kind of high 4-HBC mycobacterium genetic engineering bacteria and its construction method, and its application in the microbial fermentation preparation 22-hydroxy-23, 24-bis-norcholesta-4-en-3-ketone of 4-HBC.The high 4-HBC mycobacterium genetic engineering bacteria is constructed as follows: with mycobacterium as chassis, kshA1, kshA2, kstD1, kstD2, kstD3 gene is knocked out in turn, hsd4A gene is knocked out, ltp3, ltp4 gene is overexpressed, and the high 4-HBC mycobacterium genetic engineering bacteria is obtained.The genetic engineering bacteria provided in the present application can produce 4-HBC, greatly improve the production efficiency of steroidal drugs, help to improve the conversion rate of substrate, reduce production cost, and reaction condition is mild, environment-friendly, suitable for vigorous popularization and application, with higher economic benefit and social benefit.

This invention discloses a method for the kinetic resolution of oxaspirone via organocatalytic hydrogenolysis. Using chiral phosphate CPA as a catalyst, Hantzsch ester as a hydrogen source, and racemic oxaspirone 2,4-dien-6-one rac-1 as a substrate, a series of axially chiral biaryl phenolic compounds 2 are synthesized via asymmetric hydrogenolysis, and the central chiral oxaspirone 1 is recovered. This invention offers advantages such as simple and practical operation, readily available raw materials, high resolution coefficient, and good enantioselectivity. Some of the axially chiral biaryl products have structures similar to axially chiral cannabinol, possessing potential medicinal value.

This invention discloses a method for the catalytic hydrolysis of 3,3'-oxybis(cyclohexane-2-en-1-one) using carbon materials. Under the action of a bio-carbon-supported potassium-magnesium oxide catalyst rich in strongly basic sites, 3,3'-oxybis(cyclohexane-2-en-1-one) undergoes a hydrolysis reaction to produce 1,3-cyclohexanedione. The raw material 3,3'-oxybis(cyclohexane-2-en-1-one) is a byproduct of the resorcinol process for preparing 1,3-cyclohexanedione, and is inexpensive and readily available. The catalytic hydrolysis of 3,3'-oxybis(cyclohexane-2-en-1-one) to produce 1,3-cyclohexanedione achieves value-added processing of byproducts from the CHD industry, reduces solid waste generation, lowers the production cost of 1,3-cyclohexanedione, and has significant socio-economic benefits.

The present invention relates to a process for the preparation of Halogenated Alkenone Ethers of Formula (1) from a compound of Formula (2) using an iodide- based catalyst which enables superior process performance in terms of throughput, yield, and product purity when compared to the prior art, in addition to making the process more environmentally friendly by enabling the use of environmentally benign, inexpensive inorganic bases - in lieu of environmentally damaging organic bases, as were used in the prior art.

The invention relates to the technical field of microorganisms, in particular to a method for synthesizing 6 alpha, 11 alpha, 22-trihydroxy-23, 24-dinorchol-4-ene-3-ketone through microorganisms. The invention provides absidia coerulea Syph-GBC-2021-005 which is preserved in the China Center for Type Culture Collection, and the preservation number of the absidia coerulea Syph-GBC-2021-005 is CCTCC (China Center for Type Culture Collection) NO: M 2021341. The strain can efficiently convert 4-HBC to synthesize 6 alpha, 11 alpha-dihydroxy-4-HBC, and has the advantages of high conversion rate, high selectivity and high product yield. The method for synthesizing the 6 alpha, 11 alpha-dihydroxy-4-HBC by utilizing the microorganisms, provided by the invention, is high in conversion rate and short in conversion period, provides an important precursor compound for synthesis of a steroid drug, provides a new method for synthesis and development of the steroid drug, and has a relatively good application prospect.

Disclosed herein are compounds of the formulas:as well as analogs thereof, wherein the variables are defined herein. Also provided are pharmaceutical compositions thereof. In some aspects, the compounds and compositions provided herein may be used to inhibit RORγ and / or reduce the expression of IL-17. Also provided are methods of administering compounds and composition provided herein to a patient in need thereof, for example, for the treatment or prevention of diseases or disorders associated with inflammation or autoimmune disorders.

The present invention relates to a quinazolone enoneazole compound, its preparation method and application. As shown in general formula I, this kind of compound has certain inhibitory activity against one or more of Gram-positive bacteria and Gram-negative bacteria, can be used for preparing antibacterial drugs, and has no obvious drug resistance. Moreover, the preparation raw materials are simple, cheap and easily available, which has important significance for the application in the aspect of anti-infection.

The application discloses a synthetic method of preparing a plant source cholesterin key intermediate 20-formyl-pregn-4-ene-3-ketone. The method takes plant source 21-hydroxy-20-methyl-pregn-4-ene-3-ketone, also known as bisnorol or BA, as raw material, and oxidizes BA into aldehyde through a phase transfer catalyst under oxygen environment. The preparation method has the advantages of high yield, mild reaction condition, fast reaction time, cheap and recyclable solvent, relatively simple operation and the like, solves the problems of high production cost and serious pollution in the prior art, has high industrial production value and good agricultural application prospect, and provides a new method for synthesizing medicinal auxiliary materials of plant source cholesterin. The reaction formula is as follows.

The present application relates to the technical field of organic synthesis, in particular to a synthesis method of polysubstituted pyrazole compounds, which comprises adding aryl diazonium salt 0.6 mmol, enone 0.9 mmol, 0.5 ml of acid and 0.3 mmol of electrolyte into a 10 ml three-necked bottle, and then adding 6 ml of solvent to dissolve; using a carbon rod as an anode and a platinum plate as a cathode, stirring the reaction, monitoring the reaction process by using thin layer chromatography, after the reaction is completed, extracting the mixture with ethyl acetate; drying the organic layer of the mixture with anhydrous sodium sulfate, rotary evaporating the solvent under reduced pressure, purifying the residue by column chromatography, and obtaining the target product; the method uses aryl diazonium salt as a double synthetic substrate under mild electrochemical conditions, continuously generates two free radicals by electrochemical reduction of aryl diazonium salt, directly synthesizes a series of polysubstituted pyrazole compounds, directly and orderly constructs polysubstituted pyrazole compounds without transition metal or external redox agent, is environment-friendly, efficient and high in atom economy.

The present invention relates to a chiral iridium hydride complex comprising a) a chiral (P, N)-ligand and b) a stabilized ketene ligand of formula (I), wherein R1 is selected from the group consisting of hydrogen, a C1-C500-alkyl group, a C2-C500-alkenyl group, a C1-C500-alkoxy group, a C2-C500-alkenyloxy group, a C1-C500-alkylamino group, a C2-C500-alkenyl amino group, a di-(C1-C500-alkyl) amino group, a di-(C2-C500-alkenyl) amino group, a N-(C1-C500-alkyl)-N-(C2-C500-alkenyl) amino group, a C3-C8-cycloalkyl group, a C3-C8-cycloalkyloxy group, a C3-C8-cycloalkylamino group, a N-(C1-C500-alkyl)-N-(C3-C8-cycloalkyl) amino group, and a pharmaceutically acceptable salt thereof; a C6-C14-aryl group, which may be substituted as further defined in the specification; r1a is selected from hydrogen, C1-C6-alkyl, C1-C6-alkylcarbonyl, or R1a and R1 together with the carbon atom to which R1a is attached and the carbonyl to which R1 is attached form a C5-C7-cycloalkanone ring wherein the C5-C7-cycloalkanone ring is unsubstituted or substituted by 1 to 4 substituents independently selected from C1-C6-alkyl and benzylidene, wherein the benzylidene group is unsubstituted or substituted by 1 to 5 substituents independently of one another selected from the group consisting of halogen, a C1-C500-alkyl group, a C1-C500-alkoxy group, a C1-C500-haloalkyl group, and a C1-C500-haloalkoxy group; r2 is selected from hydrogen, a C1-C500-alkyl group, a C1-C500-alkoxy group, a C1-C500-alkylamino group, a di-(C1-C500-alkyl) amino group, a C3-C8-cycloalkyl group, a C3-C8-cycloalkyloxy group, a C3-C8-cycloalkylamino group, an N-(C1-C500-alkyl)-N-(C3-C8-cycloalkyl) amino group, a C6-C14-aryl group, which may be substituted as further defined in the specification; and arrow represents a bond attached to an iridium atom; the present invention relates to chiral iridium hydride complexes, and to a method for producing optically active 4-substituted 1, 2, 3, 4-tetrahydroquinolines by enantioselective hydrogenation of the corresponding 4-substituted 1, 2-dihydroquinolines in the presence of such chiral iridium hydride complexes.

The invention discloses a method for preparing 3 beta-hydroxy-androstane-5-ene-17-ketone-D6 (abbreviated as dehydroepiandrostene-D6) from androstane-4-ene-3, 17-diketone-D8 (abbreviated as androstenediketone-D8), and the dehydroepiandrostene-D6 is prepared from the androstenediketone-D8 as a raw material through five steps of enol esterification, upper protection, reduction, deprotection and deuterium hydrogen replacement. According to the preparation method, androstenedione-D8 is taken as a raw material, enol esterification is firstly carried out, then 17-carbonyl is subjected to ethylene glycol protection, 3-carbonyl is reduced through sodium borodeuteride under the condition of a deuterated solvent, deuterium atoms are introduced to the 3-position and the 4-position respectively, then ethylene glycol protection is removed, finally deuterium hydrogen replacement is carried out, the deuterium atom at the 16-position is replaced with a hydrogen atom, and the androstenedione-D8 is obtained. And the dehydroepiandrosterone D6 is prepared and obtained. The method disclosed by the invention is mild in reaction condition and simple to operate, can realize efficient preparation of dehydroepiandrosterone D6, and has an important application prospect.

The invention discloses a detoxification agent as well as a preparation method and application thereof, the preparation method comprises the following steps: (1) crushing cleaned and dried shrimp shells and / or crab shells, soaking with hydrochloric acid, centrifuging to obtain a first precipitate, and finally washing and drying the first precipitate to obtain a first dried substance; (2) performing firing, grinding, ultrasonic treatment and centrifugal treatment on the first dried substance to obtain a second precipitate, and then washing and drying the second precipitate to obtain a second dried substance; and (3) performing firing, ultrasonic treatment and centrifugal treatment on the second dried substance to obtain a third precipitate, and then washing and drying the third precipitate to obtain the detoxification agent. The detoxification agent disclosed by the invention can be used for efficiently removing harmful substances such as zearalenone and / or benzo [a] pyrene and the like.

The invention discloses a compound and a preparation method thereof, a perovskite solar cell, a power utilization device and a power generation device, the compound is used for an electron transport layer of the perovskite solar cell, the compound comprises a fullerene pyrrolidine group and an R group connected with the fullerene pyrrolidine group, the R group comprises an alkane group and a halogen group, and the halogen group is a halogen group. The alkyl group is at least one of an ether group, a sulfonyl group, a phosphoryl chloride group, a halogen ether group, a ketene group, an amide group and an amino ester group. The invention provides a new material capable of being used for an electron transport layer, and the perovskite solar cell containing the electron transport layer of the compound provided by the invention has the photoelectric conversion efficiency basically equal to or better than that of a perovskite solar cell with an electron transport layer formed by an electron transport material in related technologies. The compound has a relatively high oil-water distribution coefficient, and is beneficial to preparation of large-size perovskite solar cells.