51 results about "Formylation" patented technology

A method for producing a higher alcohol from a waste plastic feedstock is disclosed, comprising: (a) providing a hydrocarbon feed stream comprising a pyrolysis oil feed obtained from pyrolysis of plastic waste, wherein the pyrolysis oil comprises at least 20 wt % higher olefins with a carbon number in the range C5-C20, based on its total hydrocarbon content; (b) contacting the hydrocarbon feed stream with synthesis gas under hydroformylation conditions in the presence of a hydroformylation catalyst and recovering a hydroformylation product; (c) subjecting the hydroformylation product to hydrogenation and / or a distillation to recover a higher alcohol product.

The application discloses a rhodium-catalyzed desymmetrization hydroformylation method for constructing polychiral center carbon ring nucleosides. The method for constructing polychiral center carbon ring nucleosides comprises the following steps: under the condition of an inert atmosphere, an acetylacetone dicarbonyl rhodium metal precursor and a chiral ligand are added into an organic solvent to prepare a catalyst solution, the catalyst solution is mixed with a substrate, and a reaction is carried out under the condition of a hydrogen atmosphere and a carbon monoxide atmosphere; after the reaction is completed, filtration and purification are carried out, and polychiral center cycloalkyl aldehyde is obtained; and the aldehyde group is converted to obtain the polychiral center carbon ring nucleosides. The method for constructing polychiral center carbon ring nucleosides has the advantages of high selectivity, wide substrate compatibility, high reaction efficiency, easy conversion of products, and the like. The whole reaction process can obtain polychiral center cycloalkyl aldehyde in one step with extremely high enantioselectivity and diastereoselectivity, the aldehyde group is converted, polychiral center carbon rings can be obtained with high yield, high dr value and high ee value, and the method is simple and easy to operate.

The invention discloses a preparation method of methoxy imidazo [1, 5-a] pyridine, which comprises the following steps: firstly, taking a compound P1, specifically 1-methylamino-3-methoxypyridine, as an initial raw material, and carrying out carbamylation reaction in a formylation reagent to prepare a compound P2, specifically N-[(5-methoxypyridine-2-yl) methyl]; further carrying out intramolecular ring closing reaction on the compound P2 to obtain a compound P3 which is specifically 7-methoxy imidazo [1, 5-a] pyridine; then, a selective bromination experiment at the C3 position is carried out by taking a compound P3 as a parent skeleton and cyanogen bromide (CNBr) as a bromination reagent, and finally, specific bromination of the C3 site of the imidazo [1, 5-a] pyridine with the selectivity of 100% is realized. A solid theoretical basis is laid for efficient specific modification of the low-reaction-activity C3 site, and an efficient synthesis path is provided for rapid construction of the imidazopyridine derivative, so that the imidazopyridine derivative has a wide application prospect.

The application discloses a synthesis method of aromatic aldehyde, comprising the following steps: under inert atmosphere, a compound shown in formula I and a compound shown in formula II are reacted in an organic solvent containing a photocatalyst, a nickel catalyst, a ligand, a base and water under blue light irradiation to obtain aromatic aldehyde shown in formula III; formula I, formula II and formula III are structures as follows, ring A is selected from benzene, pyridine, thiophene, furan, pyridazine, indazole, indole, isoquinoline, quinoline, naphthalene, benzothiophene, dibenzofuran or dibenzothiophene; the application generates formyl radicals under the nickel synergistic photo-oxidation and reduction catalytic condition, and the formylation of bromobenzene and its derivatives is realized in a simple and efficient one-pot way, aromatic aldehyde is constructed, and the reaction has the characteristics of cheap and easily available raw materials, mild reaction conditions, controllable synthesis process, high separation yield / yield, green environmental protection, wide substrate applicability and the like.

This invention belongs to the field of heterogeneous Rh-based catalyst technology, and discloses a method for preparing a heterogeneous rh-based catalyst and its application. This invention prepares a heterogeneous rh-based catalyst using a one-pot method. By employing a reduction-reoxidation process, the content of different valence states of rhino in the rhino species on the surface of the heterogeneous rh-based catalyst is simply and precisely controlled, increasing the content of the most favorable δ+ valence state from 7.31% to 44.78%, thereby giving the catalyst higher hydroformylation activity. Under reaction conditions of 120℃ and a mixed gas pressure of 2 MPa, the styrene conversion rate reaches 73.9% and the aldehyde selectivity reaches 95.9% within 4 hours, which is superior to most heterogeneous rhino-based catalysts and close to that of homogeneous rhino catalysts. The heterogeneous rhino-based catalyst is prepared by the sol-gel method, which is simple in preparation and control. The prepared catalyst has a uniform rhino distribution, stable performance, and is beneficial for industrial applications.

A catalytic one-pot process for the preparation of an alcohol is provided. The process comprises decomposition of methanol into synthesis gas, the hydroformylation of an optionally substituted alkene using said synthesis gas and hydrogenation to the corresponding alcohol. The catalyst system combines a hydroformylation catalyst and a transition metal complex catalyst.

The application provides a preparation method of 3-aryl / alkyl-beta-naphthyl ether compounds, and the preparation method comprises the following steps: reacting trimethyl orthoformate with 1,3-diaromatic propyl ketone compounds or 1-aryl-3-alkyl ketone compounds to obtain 3-aryl-beta-naphthyl ether compounds or 3-alkyl-beta-naphthyl ether compounds. The reaction condition of the application is mild, trimethyl orthoformate is cheap and easy to obtain, can be used as a methylation reagent and a carbon source for extending a carbon chain at the same time, the range of reaction substrates is wide, and the functional group tolerance is good; the reaction is efficient, the selectivity is high, the post-treatment is simple, the operation is simple, and the application is suitable for large-scale industrial production; the complex substrate prepared in advance in the traditional reaction is avoided, the metal catalyst necessary for the traditional reaction is not needed, the binaftyl alcohol precursor compounds can be prepared with high chemical selectivity, and a more simple and efficient route is provided for the olefin hydroformylation / hydroformyl esterification reaction for synthesizing bidentate ligands.

A process for preparing 4-[5-[bis(2-chloroethyl)amino]-1-methyl-1H-benzo[d]imidazol-2-yl]butyric acid alkyl ester, in which 1 mole of 4-[5-[bis(2-hydroxyethyl)amino]-1-methyl-1H-benzo[d]imidazol-2-yl]butyric acid alkyl ester is reacted with 2.0 to 2.2 moles of chloromethylenedimethyliminium chloride or more than 2.2 to 5 moles of chloromethylenedimethyliminium chloride to prepare a by-product in the form of 4-[5-[bis(2-chloroethyl)amino]-4-formyl-1-methyl-1H-benzo[d]imidazol-2-yl]butyric acid alkyl ester. The alkyl ester can be hydrolyzed to form 4-[5-[bis(2-chloroethyl)amino]-4-formyl-1-methyl-1H-benzo[d]imidazol-2-yl]butyric acid, which can be used in the pharmaceutical field.

The invention belongs to the technical field of fluorescent probes, and particularly relates to a single-molecule fluorescent probe based on a phenothiazine structure as well as a preparation method and application of the single-molecule fluorescent probe. The preparation method comprises the following steps: firstly introducing an alkyl chain to a nitrogen atom of a raw material to obtain the phenothiazine structure-based single-molecule fluorescent probe, then carrying out regioselective formylation on the raw material to obtain the phenothiazine structure-based single-molecule fluorescent probe, then treating the raw material by adopting aluminum trichloride to realize O-demethylation, and finally carrying out intramolecular cyclization reaction on the raw material and 1H-benzimidazole-2-acetonitrile to obtain the phenothiazine structure-based single-molecule fluorescent probe. The single-molecule fluorescent probe based on the phenothiazine structure prepared by the invention is compatible with orthogonal chemical reaction activity and maintains controllable electron transfer, so that different chemical events are converted into specific optical signals, and selective and mechanism specific fluorescent response to phosgene, copper ions and hypochlorite is realized.

This invention discloses a system and method for preparing 4-acetoxybutyraldehyde by hydroformylation of allyl acetate. The system includes a reaction unit, a separation unit, and a product tank connected in sequence, as well as a dynamic dehydration unit that forms a loop with the reaction unit through pipelines and pumps, a catalyst regeneration unit connected to the organic phase outlet of the heating unit, and a circulating dehydration unit connected between the catalyst regeneration unit and the reaction unit. The method employs a carbonyl metal catalytic system, using a bypass molecular sieve to dynamically adsorb the self-condensing water of the reaction. After separating the aldehyde product, the remaining organic phase is deeply dehydrated by the molecular sieve and recycled. This invention reduces the water content in the reaction system by setting up a closed-loop dehydration system throughout the entire process. Through the combined strategy of "dynamic adsorption by molecular sieve + deep dehydration of the circulating phase," it achieves multiple benefits, including "reduced corrosion, reduced highly toxic byproducts, and increased yield."

The present invention relates to a process for preparing and processing of synthesis gas, the process particularly comprising the steps of preparing a first gas stream comprises H2 and CO2; feeding said gas stream into a first reactor comprising a reverse water gas shift catalyst, wherein said gas stream is fed into the first reactor at a gas hourly space velocity (GHSV) in the range of from 1,000 to 100,000 h-1, wherein the reverse water gas shift reaction is conducted at a temperature in the range of from 650 to 1,000 °C, wherein in a time interval Δt, wherein Δt is in the range of from 1 to 60 minutes, the GHSV of said gas stream displays a gradient in the range of from 2,000 to 60,000 h-1, obtaining a second gas stream; feeding the second gas stream into a second reactor, wherein the second reactor comprises one or more of a methanol synthesis catalyst, a dimethyl ether synthesis catalyst, an oxo synthesis or hydroformylation catalyst, a Fischer-Tropsch synthesis catalyst, a formic acid synthesis catalyst, and a phosgene synthesis catalyst, obtaining a product stream.

This invention discloses a highly selective synthesis method for isovlandrin, comprising the following steps: Step S1, reacting guaiacol with a benzylating agent in the presence of an alkaline catalyst and an organic solvent to generate o-benzyloxyanisole; Step S2, reacting the o-benzyloxyanisole with a Vilsmeier-Haack reagent for formylation to obtain 3-benzyloxy-4-methoxybenzaldehyde; Step S3, mixing 3-benzyloxy-4-methoxybenzaldehyde with a 65wt%-70wt% aqueous sulfuric acid solution to perform an acid debenzylation reaction to obtain crude isovlandrin; Compared with the prior art, the yield of isovlandrin can reach up to 70% or more, and the selectivity is greatly improved.

The application relates to a preparation method of a mesotrione intermediate. S1, 3-chloro-2-methyl aniline, hydrochloric acid and pure water are placed in a reaction kettle, stirring, cooling, dropwise addition of a NaNO2 solution, after dropwise addition is completed, temperature control is carried out, CH3SNa aqueous solution is added, after dropwise addition is completed, slow temperature rising is carried out, and reaction is continuously carried out for 8 hours; extraction, water washing and distillation are sequentially carried out, and 1-chloro-2-methyl benzyl sulfide is obtained; S2, under the atmosphere of nitrogen, formylation reagent is added into a reaction kettle under the condition of 0-10 DEG C, a catalyst is dropwise added and stirring is carried out, 1-chloro-2-methyl benzyl sulfide is dropwise added, temperature rising is carried out, and 2-chloro-3-methyl-4-methylthio benzaldehyde is obtained through post-treatment; S3, under the atmosphere of nitrogen, methanol, 2-chloro-3-methyl-4-methylthio benzaldehyde and sodium tungstate dihydrate are added into a reaction kettle, hydrogen peroxide is dropwise added, the reaction temperature is controlled, and reaction is carried out, and the mesotrione intermediate is obtained through post-treatment.

The present invention relates to a method for the continuous hydroformylation of olefins with synthesis gas in the presence of a cobalt catalyst, wherein the method is automated by the use of APC control with at least three controlled variables A, B and C.

To provide a method for producing a compound suitable for use as a perfume and / or aroma having an aromatic note of musk.SOLUTION: A process for preparing a compound of formula (I) comprising the steps of: (A) etherifying a phenol derivative to obtain an allyl ether derivative; (B) Claisen rearrangement of the ether from step (A) followed by cyclisation; (C) acetylating or formylating the intermediate from step (B); wherein steps (A) and (B) are carried out in a one pot reaction. Wherein R1, R2, R3 and R4 represent hydrogen, methyl, ethyl, propyl, iso-propyl, butyl, sec-butyl, tert-butyl, iso-butyl, acetyl, formyl or SELECTED DRAWING: None

The present application relates to the technical field of catalytic synthesis, and specifically provides a catalyst and a preparation method thereof.The catalyst comprises a silicon-aluminum molecular sieve and a nickel metal supported on the surface of the silicon-aluminum molecular sieve; the silicon-aluminum ratio of the silicon-aluminum molecular sieve is 1.8-3.0; the specific surface area of the silicon-aluminum molecular sieve is 235-330 m 2 / g, the pore volume is 0.5-1.3 ml / g, and the pore size is 8-13 nm.The catalyst prepared by taking the silicon-aluminum molecular sieve as a carrier and taking a metal nitrate as an active component has good catalytic activity on mixed butene; the butene oligomerization and dimerization products obtained by catalyzing mixed butene by using the catalyst can be subjected to hydroformylation to produce high-carbon isoalcohols.

The application discloses a method for improving the yield of 5-hydroxymethylfurfural by using superhigh-pressure homogenization formylated cellulose, which comprises the following steps: mixing cellulose and formic acid, homogenizing the mixture for 5-25 times under the pressure of 600-1400 bar, performing solid-liquid separation to extract the precipitate, removing by-products by washing and drying; uniformly mixing 5-20 parts by weight of the treated cellulose, 0-1000 parts by weight of DMSO, 0-1000 parts by weight of deionized water, 25-125 parts by weight of metal ionic liquid and 0-80 parts by weight of acid, and reacting for 10-120 minutes under the temperature of 150-190 DEG C; and performing solid-liquid separation to obtain supernatant containing 5-hydroxymethylfurfural. The method for preparing formylated cellulose by performing superhigh-pressure homogenization pretreatment on the mixture of cellulose and formic acid and then catalytically converting the formylated cellulose into 5-hydroxymethylfurfural has good yield of reaction products, is simple in operation and easy to realize.

The invention provides a supported hydroformylation catalyst, a preparation method and a method for synthesizing pentacaraldehyde, and relates to the technical field of heterogeneous catalysis of homogeneous catalysts. The structural form of the supported hydroformylation catalyst provided by the invention is Rh (at) P-N / AC, Rh is an active center of the catalyst, and P-N / AC is a carrier; the AC is activated carbon; the structural formula of the P-N organic ligand is shown as a formula I to a formula IV. The supported hydroformylation catalyst provided by the invention can realize catalytic circulation of noble metals and phosphine ligands, and has high activity and C2 selectivity.

The application relates to the field of olefin catalysis, and discloses a supported cobalt-based alloy catalyst, a preparation method and application thereof, and a method for diisobutylene hydroformylation, the catalyst comprising a carrier, an active component and an additive, the carrier being SiO2, metal elements in the active component being Co, and metal elements in the additive being Ni; at least part of the metal elements in the active component form nano-alloy particles together with at least part of the metal elements in the additive, and the nano-alloy particles are loaded on the surface of the carrier. The supported cobalt-based alloy catalyst provided by the application has the advantages of simple preparation process, high catalytic activity, easy separation and recovery from a liquid phase, and potential application and industrial production.

The application discloses preparation and application of amino acid isocyanate derivative. The amino acid isocyanate derivative containing isocyanogen, carboxylate group and different side chains is prepared through esterification, neutralization, formylation, isocyanation and saponification by taking amino acid as raw material. The preparation route is simple in operation, low in raw material cost, mild in reaction condition, novel in synthesis route, high in product yield, various in product types and good in industrial conversion prospect. The prepared amino acid isocyanate derivative can be used in preparation of polyamino acid derivative or copolymer antibacterial material, so that the single type, high price and difficulty in obtaining of commercially available isocyanate is made up, the product added value is improved, the type selection of polyamino acid derivative or copolymer is expanded, and a new direction for further improving antibacterial activity is provided.

A process for producing aldehydes is disclosed, the process comprising: hydroformylating an olefin using a hydroformylation catalyst to form an aldehyde, recovering an effluent stream comprising the aldehyde, hydrogen, and the hydroformylation catalyst, passing the effluent stream through a stripper, contacting the effluent stream with a strip gas in the stripper to produce a stripped effluent stream having a lower hydrogen concentration than the effluent stream, and recovering the stripped effluent stream.

The application provides a bimetallic molecular sieve catalyst Co-M@MFI, and a preparation method thereof, which comprises the following steps: (1) dissolving metal precursors in water to obtain a metal salt solution; (2) adding a complex amine into the metal salt solution to obtain a complex solution; (3) adding an organic template into water, and then adding the complex solution to obtain a mixed solution; (4) adding a silicon source and an aluminum source into the mixed solution to form a mixed gel by stirring; (5) crystallizing the mixed gel at high temperature to obtain a crude molecular sieve; and (6) washing, drying, calcining, shaping and re-calcining the crude molecular sieve to obtain the bimetallic molecular sieve catalyst Co-M@MFI. In the application of the bimetallic molecular sieve catalyst Co-M@MFI in catalyzing the hydroformylation / hydrogenation reaction of olefins to generate alcohol, the coupling of the hydroformylation and the hydrogenation reaction is realized, the loss of active metal can be obviously avoided, excellent alcohol selectivity is achieved, and separation from products after the reaction is easy.

Antidegradant products are disclosed that may be made by a process comprising: hydroformylating one or more of: a fatty acid or fatty acid derivative having one or more unsaturations, e.g., carbon-to-carbon double bonds, and from 10 to 20 carbon atoms, or a fatty alcohol comprising one or more of a straight chain fatty alcohol having one or more unsaturations, e.g., unsaturated carbon-to-carbon double bonds, and from 10 to 20 carbon atoms, by reaction with carbon monoxide and hydrogen gases to obtain a hydroformylated intermediate; and functionalizing the hydroformylated intermediate by reaction with a substituted or unsubstituted paraphenylene diamine to obtain the antidegradant product.

The application discloses a method for preparing normal aldehyde by catalyzing olefins by using an oxide-molecular sieve composite catalyst. The method comprises the following steps: adding the olefins, the oxide-molecular sieve composite catalyst and a solvent into a reaction kettle, introducing synthesis gas after being closed, and obtaining a reaction product under the conditions of 80-100 DEG C, a pressure of 1-5 Mpa, a rotating speed of 800-1000 rpm and a reaction time of 0.5-3 h. The oxide-molecular sieve composite catalyst is a molecular sieve and a metal oxide which are encapsulated with an active component. The catalyst obtained by the method has high activity and stability, and the selectivity of the catalyst for linear aldehyde is remarkably improved, so that the catalyst has a good industrial application prospect.

This invention relates to a method for preparing 1,4,5,8-tetramethoxynaphthalene compounds containing the characteristic side chain of shikonin and their 6-fluoro derivatives. The method uses 2-fluoro-1,4-dimethoxybenzene or 2,5-difluoro-1,4-dimethoxybenzene as starting materials. After cyclization, ring-opening, and O-methylation to construct the 1,4,5,8-tetramethoxynaphthalene core, an aldehyde group is introduced at the 2-position via Vilsmeier-Haack formylation. This is followed by addition with allyl magnesium bromide to obtain an allyl alcohol intermediate. Finally, a cross-metathesis reaction catalyzed by a Grubbs II catalyst is performed with 2-methyl-2-butene to construct the characteristic side chain of shikonin –CH(OH)CH2CH=C(CH3)2. This invention offers high yields, simple operation, avoids the use of highly toxic reagents, and successfully solves the problem of the difficulty in synthesizing 6-fluoro derivatives due to direct fluorination, providing a key intermediate for the development of novel naphthoquinone drugs.

This invention discloses a silicon-containing monophosphine ligand, its preparation method, catalytic composition, and applications, belonging to the field of organic synthesis and catalysis technology. Addressing the problems of existing cobalt-based olefin hydroformylation systems, such as difficulty in effectively controlling the ratio of n-alcohol to iso-alcohol in the products, limited freedom in ligand structure design, and insufficient system stability and scale-up applicability, the silicon-containing monophosphine ligand of this invention can be prepared by coupling a Grignard reagent with a phosphine chloride. Furthermore, the cobalt-phosphine catalytic system composed of the silicon-containing monophosphine ligand and a cobalt precursor can achieve the direct conversion of various olefins to their corresponding alcohols under a CO / H2 atmosphere. By adjusting the structural parameters of the ligand, the ratio of n-alcohol to iso-alcohol in the products can be effectively controlled. This catalytic system exhibits good thermal stability and applicability during the reaction process, making it suitable for the industrial application of one-step preparation of higher alcohols from various olefins.

The application belongs to the technical field of hematin quantitative detection, and specifically discloses application of methylene blue cyclopropyl formylated derivative as a chromogenic substrate for detecting hematin, and uses methylene blue cyclopropyl formylated derivative AMB as a chromogenic substrate for detecting hematin Hemin; compared with a classical substrate TMB, the methylene blue cyclopropyl formylated derivative AMB of the application has higher sensitivity in the detection of hematin Hemin; in addition, the amino protons of the methylene blue cyclopropyl formylated derivative AMB of the application are fully substituted by methyl, which inhibits the participation of active oxygen free radicals in oxidation, but is still sensitive to the oxidation pathway of ferric free radicals, has better selectivity compared with TMB, and the AMB system can effectively detect hematin Hemin in a serum sample. Therefore, it can be said that for the detection of hematin Hemin, AMB is a more excellent colorimetric substrate than TMB.

The invention discloses a preparation method of a catalyst for synthesizing isomeric alcohol, and the preparation method comprises the following steps: S1, dissolving cobalt salt, copper salt and a carrier with high specific surface area in a solvent through ultrasonic dispersion, mixing, dipping, stirring, and aging to obtain a precipitate; s2, stirring and refluxing the precipitate and a 2-methylimidazole solution together, aging again, washing with absolute ethyl alcohol, and drying to obtain a catalyst precursor; and S3, calcining the catalyst precursor twice in different gas atmospheres to obtain the catalyst for synthesizing the isomeric dihydric alcohol. The catalyst prepared by the method is used for carrying out molecular addition on synthesis gas (CO + H2) and formaldehyde through a formaldehyde hydroformylation route to obtain isomeric dihydric alcohol, has the advantages of high product selectivity, good catalytic activity, environmental protection, low price and the like, can improve the selectivity of isomeric dihydric alcohol synthesis reaction, and is suitable for industrial production. The ever-increasing requirements of the chemical fiber field on low-cost and high-performance polyester raw materials are favorably met.

The present application relates to the chemical technology field, specifically to a method for synthesizing vanillin and ortho-vanillin by one-step method, which uses o-methoxyphenol as starting material, and carries out one-step reaction with formaldehyde under the action of composite catalyst, and then separates vanillin and ortho-vanillin by post-treatment of the reaction solution. By using the composite catalyst with specific composition, the present application realizes high-selectivity formylation of formaldehyde at the ortho position of the hydroxyl group of o-methoxyphenol, increases the generation proportion of ortho-vanillin from the source, avoids the use of toxic reagent, and has mild reaction conditions. By using the difference in solubility of specific mixed solvent system and adjusting the temperature, the present application can efficiently separate vanillin and ortho-vanillin, and solves the separation problem caused by the similar properties of isomers in the prior art. The overall process is simple and efficient, and the yield and product purity are significantly improved, which has excellent industrial application prospect.