98results about "Hydroxy group formation/introduction" patented technology

The invention belongs to the field of material preparation and chemical engineering, and particularly relates to an N-doped modified MOFs (Metal-Organic Frameworks) derived core-shell nanoreactor as well as a preparation method and application thereof. The preparation method comprises the following steps: taking cobalt as a node metal, synthesizing an N-doped modified MOFs material with an organic ligand and a nitrogen source through a hydrothermal reaction, then coating the surface of the material with porous silicon dioxide, and preparing the N-doped modified MOFs derived core-shell nanoreactor through a two-step calcination method. The MOFs derived core-shell nanoreactor prepared by the invention has a large specific surface area, a rich pore structure and excellent catalytic activity and stability, and is high in catalytic activity, good in recycling stability and suitable for large-scale popularization and application when being used as a catalyst for alpha, beta-unsaturated aldehyde transfer hydrogenation.

The invention discloses a synthetic method for preparing corresponding hydroquinone through normal-pressure hydrogenation of quinone. Hydroquinone is an important compound, widely exists in natural products with biological activity, and is an important precursor for synthesizing various medicines, agricultural chemicals, polymers and functional materials. The method for reducing the quinone compound into hydroquinone is a simple and direct method. Although many reducing agents, such as SnCl2, Zn, Fe, Na2S2O4, NaBH4, polymethylhydrosiloxane (PMHS), have been used for this conversion, these processes are often affected by the use of stoichiometric or excess reagents, violent reaction conditions, and the formation of large amounts of waste. The hydrogenation reaction of quinone with H2 is obviously the most ideal way to achieve this conversion because it has high atomic efficiency and environmental friendliness. However, hydrogenation often needs high-pressure equipment or high temperature, so that the application potential is greatly limited. Accordingly, we we wish to exhibit a process for the hydrogenation of quinone to hydroquinone under atmospheric pressure.

The invention provides a method for high-yield recovery of phenolic compounds from epoxy resin-based waste, which comprises the following steps: mixing epoxy resin with acid / acid solution and salt according to a mass ratio of 1: (5-100): (0.1-50), reacting at 30-300 DEG C for 0.5-60 hours, collecting the reaction product, and separating to obtain a liquid product, and separating, purifying and recovering the liquid product to obtain the phenolic compound. According to the method, the acid / acid solution and the salt are creatively utilized to synergistically degrade the epoxy resin material, and particularly, the yield of the phenolic compounds in the degradation product can be remarkably improved under the conditions of specific combination, specific proportion and reaction, so that a new way is provided for recovering the phenolic compounds from the epoxy resin-based waste through a chemical method; the industrial application is expected to be realized.

The invention discloses a metal-free catalyst, a preparation method and application of the metal-free catalyst in preparation of benzyl alcohol through transfer hydrogenation of biomass-based benzaldehyde, and the catalyst is a nitrogen-doped carbon catalyst; in the catalyst, nitrogen is used as a Lewis alkaline site, and does not contain a Lewis acidic site and a # imgabs0 # acidic site. According to the preparation method of the metal-free nitrogen-doped carbon-based catalyst, the metal-free nitrogen-doped carbon-based catalyst (MF-NC) can be prepared through solvothermal self-assembly and pyrolysis processes by virtue of a structure regulator and taking a ZIF material as a sacrificial template, the preparation process is simple, the surface appearance is controllable, and the metal-free nitrogen-doped carbon-based catalyst has a relatively high specific surface area. The obtained MF-NC can efficiently and selectively convert benzaldehyde into benzyl alcohol through a Lewis alkaline site mediated MPV transfer hydrogenation reaction by taking cheap and renewable bioethanol as an in-situ hydrogen donor and a reaction solvent.

The present application relates to a kind of catalyst composition and its application in catalytic preparation optically active secondary alcohol, the catalyst composition includes chiral ionic bridged aryloxyalkane rare earth complex and additive, the additive is selected from one or more of pyrimidine, N,N-dicyclohexylmethylamine, 4,4'-dipyridyl.The above-mentioned catalyst composition can be used for synergistically catalyzing asymmetric borohydration of chalcone and its derivatives with pinacol borane, and show high catalytic activity and high enantioselectivity, product yield is as high as 99%, ee value can reach 84%, provide a reliable new way for the efficient, high selective synthesis of optically active secondary alcohol.

The invention discloses a method for preparing monophenol compounds from lignin. The method comprises the following steps: mixing a raw material lignin with a solvent, and carrying out a one-step hydrogenation reaction in a hydrogen atmosphere under the action of a nickel-molybdenum-based catalyst to prepare the monophenol compound, the nickel-molybdenum-based catalyst comprises metal nickel and nickel oxide, molybdenum oxide and silicon oxide. The method provided by the invention has the characteristics of low production cost, simple separation, high monophenol compound yield and the like.

The present invention relates generally to methods for producing detergent compounds from waste plastic feedstocks. More specifically, the invention relates to methods for producing detergent intermediates, including alkylbenzenes, paraffins, olefins, oxo alcohols, and surfactant derivatives thereof from waste plastic feedstock.

The present invention discloses a method for realizing allylic C-H alkylation reaction by a LMCT process involving light-induced metal chromium. In the presence of a chromium catalyst and under the irradiation of blue light: (a) compound 1 reacts with compound 2, 4 or 6 to generate compound 3, 5 or 7; or (b) compound 8 undergoes an intramolecular reaction to generate compound 9. The present invention realizes the LMCT process involving metal chromium under light-induced conditions for the first time. The C-H alkylation method provided does not require additional photosensitizers and HAT reagents, has 100% atom economy, and the reaction can occur smoothly both intramolecularly and intermolecularly. The method provided by the present invention has the advantages of cheap and readily available reaction raw materials, simple reaction operation, wide application range of reaction substrates, easy reaction amplification, mild reaction conditions, etc., and can realize industrial production and application.

The application belongs to the technical field of chemical synthesis, and specifically provides a chiral hydroxyphosphonate, a preparation method and application thereof. The chiral hydroxyphosphonate has a structure as shown in formula II: each R is independently H, an alkyl group, an alkenyl group, an alkynyl group or a halogenated alkyl group; Ar is an aromatic ring or a heteroaromatic ring; X is a bond, -O-, -N(R 1 )- 2 q , -S(=O) m -; the chiral hydroxyphosphonate is obtained by reducing an alpha phosphonate substituted benzocycloalkanone compound through an asymmetric hydrogenation method, has two chiral centers, and has a yield of up to 99% and an enantiomeric selectivity of up to 99%. The chiral hydroxyphosphonate has wide application potential and value in skin tissue soothing, repairing, anti-aging and the like.​

The application belongs to the technical field of chemical synthesis, and particularly relates to a method for asymmetrically synthesizing adjacent halogenated alcohol compounds. The cis adjacent halogenated alcohol compound is prepared through catalytic hydrogenation of asymmetric dynamic kinetic resolution of alpha halogenated ketone. The method has mild reaction conditions, excellent enantiomer and diastereomer selectivity, high efficiency and good yield, and has good application prospect.

[Abstract] [Problem] To provide a method for producing a dealkoxyphenylation product with high yield from a substrate, e.g., a sugar, which is bonded to an alkoxyphenyl group through an oxygen atom. [Solution] A substrate that is bonded to a phenyl group substituted by a C1 to C5 alkoxy group at a para- or ortho-position through an oxygen atom is reacted with a λ3-iodane in a fluorous alcohol and water, whereby a dealkoxyphenylation product can be obtained with high yield under mild conditions.

The invention discloses a continuous flow preparation method of polysubstituted propargyl alcohol, which uses a microtube continuous flow reaction device and comprises the following specific steps: simultaneously conveying acetylene gas or terminal alkyne compound and an organic alkali solution into a mixer for premixing; simultaneously conveying the keto-carbonyl substrate and the flowing-out reaction liquid to a reactor to carry out an alkyne hydrogenation reaction; and carrying out gas-liquid separation on the outflowing reaction liquid, and rectifying in a rectifying tower to obtain a target propargyl alcohol product. According to the method for continuously preparing the polysubstituted propargyl alcohol by using the continuous flow reaction system, full mixing of reaction materials of each reaction unit and accurate control of the reaction can be realized by regulating and controlling pipeline parameters, the automation degree is greatly improved, the manual operation is reduced, the energy consumption cost is reduced, and the method is suitable for industrial production.

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 present disclosure relates to the field of alternative methods to form alkynols and / or acetylene alcoholates. In a first aspect, the present disclosure concerns a method comprising the steps of i) providing a mixture comprising a solvent, 1,2-dibromoethane, a carbonyl compound and an alkali hydroxide, and ii) allowing the 1,2-dibromoethane, the carbonyl compound and the alkali hydroxide to react at a reaction temperature forming a reaction mixture, wherein the solvent comprises at least 85 wt% dimethyl sulfoxide.

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 application discloses a novel zirconium-nitrogen coordination polymer catalyst, which has a porous structure and is prepared by a coordination self-assembly method at normal temperature from zirconium ions and non-cyclic nitrogen-containing organic ligands, only introduces Lewis acid-base sites, and does not introduce Brønsted acid sites. The presence of the Lewis acid-base sites can efficiently catalyze MPV transfer hydrogenation reaction of biomass-based aldehyde ketone compounds, the absence of the Brønsted acid sites can avoid side reactions such as etherification and acetalization, and the porous structure can greatly promote the mass and heat transfer processes during the reaction, and the synergistic effect between them further improves the yield and selectivity of the target product.

The present disclosure relates to a method for olefin oxygen oxidation, comprising the following steps: contacting an olefin compound with a catalyst under oxygen condition to perform an oxidation reaction; the catalyst is a composite catalytic material, the composite catalytic material comprises a framework heteroatom molecular sieve and a metal element M dispersed in the intracrystalline of the molecular sieve; the framework heteroatom molecular sieve is a molecular sieve in which at least part of silicon in a full-silicon molecular sieve framework is replaced by a heteroatom element Q, and the heteroatom element Q is selected from one of titanium, boron, zirconium, aluminum, tin, phosphorus and germanium. The method uses a metal-containing multi-level porous heteroatom molecular sieve for olefin oxygen oxidation reaction, and high conversion rate of olefin and high selectivity of ketone and dihydroxyl compound can be obtained under relatively mild conditions.

The present invention discloses a hydrogenation catalyst, a method for preparing the catalyst, and an application thereof. The method for preparing the hydrogenation catalyst comprises: dissolving an organic ligand in a first organic solution to obtain a ligand solution; dissolving a zinc salt in a second organic solution to obtain a zinc salt solution; adding the zinc salt solution to the ligand solution under stirring to carry out a coordination reaction to obtain a crude precursor; vacuum drying the crude precursor to obtain a precursor; and calcining the precursor to obtain the catalyst. The catalyst prepared by this method is particularly suitable for the preparation of cinnamyl alcohol by transfer catalytic hydrogenation of cinnamaldehyde, has a high cinnamyl alcohol hydrogenation conversion rate and cinnamyl alcohol selectivity, and has certain cyclic stability.

This invention discloses a chiral monophosphine ligand, its preparation method, and its application in asymmetric synthesis. The ligand preparation method involves mixing an N,N',1,2-tetrasubstituted ethane-1,2-diamine compound, phosphorus trichloride, triethylamine, and solvent under a nitrogen or argon atmosphere at -80 to -70°C, and reacting at 60 to 80°C for 6 to 8 hours. The resulting reaction mixture is then cooled to room temperature, and an alcohol, phenol, or Grignard reagent is added dropwise, reacting at 60 to 80°C for 8 to 12 hours. The resulting mixture is then post-treated to obtain the chiral monophosphine ligand. The application involves stirring a nickel catalyst, a chiral monophosphine ligand, a solvent, a diene, and an aldehyde under an argon or nitrogen atmosphere at a specified temperature for 12 to 15 hours. The mixture is then post-treated to obtain the target product. This method utilizes widely available and inexpensive raw materials, and the operation is simple, achieving high stereoselectivity and enantioselectivity in the synthesis of alcohol compounds containing chiral conjugated dienes through a one-step reaction.

The invention comprises chiral aminophosphine ligands of the formula I, iridium catalysts containing the chiral aminophosphine ligands of the formula I, of the formula II or III;, and the use of the iridium catalysts in the asymmetric hydrogenation of a compound, containing at least one prochiral keto group preparation and the formation of chiral alcohols.

The invention belongs to the technical field of organic synthesis, and particularly relates to a universal selective co-production method of monosubstituted alkynyl tertiary alcohol, which comprises the following steps: 1) adding alkali and an organic solvent into a reaction container, replacing air in the reaction container with acetylene gas, and continuously introducing the acetylene gas into the reaction container to keep the acetylene pressure in the reaction container at 0.10-0.25 MPa; 2) stirring and heating to 20-80 DEG C, dropwise adding ketone into the reaction container, and carrying out heat preservation reaction until the reaction is finished; and 3) quenching the reaction liquid, taking an organic phase material, washing, drying, and carrying out rotary evaporation concentration to obtain the target product. Acetylene and ketone are used as raw materials for co-production of the monosubstituted alkynol and the disubstituted alkynol, the yield of the monosubstituted alkynol can reach 24.86% at most, and the method is suitable for various ketone compounds and has good universality, and the process is simple to operate and easy to industrially popularize.

The application discloses a metal complex and a preparation method and application thereof. Specifically, the metal complex catalyst is prepared by complexing a chiral tetradentate ligand with a metal precursor, the catalyst can realize asymmetric hydrogenation of a ketone, and through comparison of different preparation catalyst processes, an easy-to-prepare and simple-to-operate method is determined, the metal complex catalyst prepared by the method is stable in property, has certain tolerance to water and oxygen, can greatly improve catalytic efficiency, is suitable for industrial production, has a wide substrate application range, and has important practical value and industrialization prospect.

A selective hydrogenation process is disclosed that can upgrade impure feeds, such as those obtained from biomass containing several small (e.g., 2-6 carbon atoms) molecules with aldehyde and / or ketone carbon atoms. For example, glycolaldehyde and its methylated derivative, hydroxyacetone (acetol), are both high-value intermediates for certain downstream processing reactions, but they are typically recovered in the condensate from the pyrolysis of carbohydrates (e.g., aldose-containing sugars) along with glyoxal and its methylated derivative, pyruvaldehyde. Selective hydrogenation of compounds with two carbonyl carbon atoms without overhydrogenation to ethylene glycol and propylene glycol can increase the concentration of desired intermediates. The beneficial effects of such selective hydrogenation can be achieved through the use of hydrogenation catalysts containing precious metals, such as Ru and Pt.

The invention relates to a preparation method of a rhodium-phosphine complex catalyst. The preparation method of the rhodium-phosphine complex catalyst comprises the following steps: providing an alcoholic solution of a bidentate phosphine ligand; in an inert gas atmosphere, sequentially dropwise adding an alcoholic solution of rhodium trihalide hydrate and a formaldehyde solution into the alcoholic solution of the bidentate phosphine ligand to obtain a premixed solution; and heating the premixed solution to a predetermined temperature, and reacting for a predetermined time to obtain the rhodium-phosphine complex catalyst. Wherein the bidentate phosphine ligand is one of molecules represented by a general formula (1): # imgabs0, R1 is selected from one of groups represented by a general formula (2.1), a general formula (2.2), a general formula (2.3) and a general formula (2.4): # imgabs1 # Ar1, Ar2, Ar3 and Ar4 are all aryl groups. The method is simple and easy to operate, the problem of tedious process does not exist, and the high yield of about 95% is achieved.

The application provides a kind of chiral P, N, N ligand and its preparation method and application in asymmetric hydrogenation reaction. 2-diphenylphosphinyl phenethylamine is mixed with 6-phenylpyridine-2-formaldehyde, nitrogen is filled, methanol is added, the formed mixture is refluxed, after cooling, NaBH4 is added. Then, the mixture is refluxed again. Cooling, water is added, dichloromethane is extracted, anhydrous sodium sulfate is dried, after removing solvent, the desired chiral P, N, N ligand is obtained by column chromatography. The catalyst formed by the chiral ligand described in the application and Mn, Ir-, Ru- and other metal precursors has excellent catalytic activity and stereoselectivity in the catalytic asymmetric hydrogenation reaction of C=C, C=N and C=O double bond. The enantioselectivity is as high as 99% ee, and the TON is as high as 100000.

Process for the ruthenium-catalysed hydrogenation of aldehyde acetals.

The present application relates to a kind of light-induced synthesis method of chromium-catalyzed beta-deuterated alcohol, the present application uses alpha-deuterated alkyl sulfonium salt, aldehyde as reaction raw material, chromium salt as catalyst, adds Hantzsch ester, with tetrahydrofuran as reaction solvent, under the irradiation of 400-410nm blue light, room temperature stirring reaction 12h.After reaction, a series of beta-deuterated alcohol with higher deuterium content is obtained, the reaction condition is mild, easy to operate, provides reliable experimental method for synthesis of deuterated molecule, has good industrial application prospect.

The invention provides a synthesis method and application of an arylamine and indole compound containing a hexafluoroisopropanol structural unit, and the synthesis method comprises the following steps: dissolving hexafluoroacetone trihydrate and an arylamine compound or an indole compound in an organic solvent to directly react for 6-48 hours at the reaction temperature of 10-100 DEG C; and after the reaction is finished, carrying out post-treatment to obtain the arylamine and indole compound containing the hexafluoroisopropanol structural unit. The method has the advantages of mild reaction conditions, simple operation, cheap and easily available raw materials, high atom economy, good functional group compatibility, wide substrate application range (can be directly used for later derivatization of some drug molecules), no waste generation, and suitableness for industrial production. The synthesized arylamine and indole compound containing the hexafluoroisopropanol structural unit can be used as an organic molecular catalyst to be applied to a hydroxydifluoroalkylation reaction of indole and difluoroacetaldehyde hemiethanol, and shows better reaction activity.

The invention relates to the technical field of organic chemical synthesis, and discloses a preparation method of a beta-aryl arylacetone compound. The chemical structural formula of the beta-aryl arylacetone compound is shown as a formula (I), the method comprises the following steps: in the presence of a protective gas, an organic solvent and a catalyst, water and a chalcone compound shown as a formula (II) are subjected to a hydrogenation reduction reaction, and a component A is sodium sulfide and / or sodium sulfide nonahydrate. The preparation method provided by the invention has the advantages of mild reaction conditions, high yield, simplicity and convenience in operation, no need of metal and the like.