516 results about "Palladium catalyst" patented technology

The invention belongs to the technical field of catalytic oxidation of carbon-containing industrial waste gas, and particularly relates to a Pd catalyst for catalytic combustion of carbon-containing waste gas as well as a preparation method and application of the Pd catalyst. The invention provides a Pd catalyst for catalytic oxidation of carbon-containing industrial waste gas such as CO and volatile organic pollutants VOCs. The Pd catalyst is obtained by compounding an amorphous CeO2 nano-cluster with a TiO2 substrate (marked as cCeO2 / TiO2) and indirectly regulating the form of Pd through gradient regulation of the content of the amorphous CeO2 nano-cluster by a sol-gel method on the basis of strong interaction of Pd and Ce species. The Pd catalyst prepared by the invention shows excellent low ignition temperature, high performance and certain universality in the catalytic combustion process of carbon-containing industrial waste gases such as CO and low-chain VOCs (Volatile Organic Compounds). In addition, the method for preparing the Pd catalyst is simple to operate and mild in condition, and has great industrial application potential and value.

The invention discloses a palladium catalyst as well as a preparation method and application thereof. The structural formula of the palladium catalyst is shown as a formula (I), according to the invention, an alkoxy group is introduced into the skeleton of the palladium catalyst and N-methylimidazole is coordinated with palladium, so that the catalytic yield of the palladium catalyst is effectively improved, and long-chain alkyl polyarylamine with high molecular weight and narrow distribution is obtained; the method does not need to use a traditional phosphine ligand, avoids potential hazards of phosphine compounds to operators and the environment in the use process, and is expected to be industrially applied on a large scale due to the fact that the phosphine compounds are stable to air and moisture and can be stored for a long time.

The invention belongs to the field of preparation of halogen-containing substituted benzoic acid, and particularly relates to a method for preparing o-chlorobenzoic acid through hydrogenation selective debromination. According to the invention, hydrogen is used as a reducing agent, a palladium catalyst is used as a catalyst, a methanol aqueous solution is used as a solvent, and 2-chloro-3-bromobenzoic acid, 2-chloro-5-bromobenzoic acid or a mixture thereof are used as raw materials to prepare o-chlorobenzoic acid. According to the method, debromination is controlled through selective hydrogenation instead of dechlorination, so that generation of a byproduct benzoic acid is inhibited. The scheme is reasonable in design, simple in process and mild in reaction condition, and a new thought is provided for the synthesis method of o-chlorobenzoic acid.

The present invention relates to the technical field of organic synthesis, and specifically relates to a method for constructing the chirality of a pyran ring in Orforglipron by means of enzymatic catalysis, the method comprising the following steps: step S1, by using SM1 and SM2 as starting materials, carrying out a reaction under the action of a palladium catalyst and a ligand to obtain INT-1; step S2, under the catalysis of Pd / C, subjecting INT-1 to double bond hydrogenation reduction to obtain INT-2; step S3, in the presence of a solvent, a buffer salt system and enzymatic catalysis, subjecting INT-2 to hydrolysis and resolution to obtain a chirally pure intermediate INT-3; step S4, subjecting INT-3 to a Grignard reaction for cyclization, so as to synthesize a lactone intermediate INT-4; and step S5, subjecting INT-4 to reduction by means of Dibal-H, quenching same, performing extraction with dichloromethane, drying same with anhydrous sodium sulfate, and then performing reduction by means of triethylsilane to obtain a compound of general formula A. In the present invention, the chirality is constructed by means of enzymatic catalysis without the need of SFC resolution for separating isomeric impurities during the construction of the chirality, thereby reducing losses and improving yield, obtaining the target product at high yield and high chiral selectivity, and further saving expenses and reducing costs.

The invention discloses a hydrogen-fluorine atom doped graphdiyne material and a preparation method thereof, and relates to the technical field of carbon materials. According to the method, halogenated aromatic hydrocarbon and an alkynyl compound are taken as raw materials, a palladium catalyst and a copper catalyst are taken as a catalytic system, and an acetylenic bond of the alkynyl compound and the halogenated aromatic hydrocarbon are subjected to a Sonogashira coupling reaction to obtain the hydrogen-fluorine-doped graphite alkynyl material. The graphdiyne material provided by the invention has a large pore diameter, multiple active sites and high thermal stability and chemical stability, so that the hydrofluorine-doped graphdiyne material has excellent electrochemical energy storage property, shows reversible capacity of 1155mAh g <-1 > under 0.05 Ag <-1 > when being used as a negative electrode of a lithium ion battery, and can be used as a negative electrode of the lithium ion battery. And the density is almost 3 times that of a commercial graphite negative electrode material (300-350mAh g <-1 >). The application of the graphdiyne material in the field of electrochemical energy storage is obviously promoted.

The invention provides a catalyst as well as a preparation method and application thereof and a preparation method of tetrahydrofurfuryl alcohol, the catalyst takes mesoporous silica as a carrier, the surface of the carrier is modified with polyethylene glycol and an alkyl chain to form an amphiphilic surface, and Pd nanoparticles are loaded in mesopores. The surface of the mesoporous silica supported palladium catalyst is modified with polyethylene glycol and alkyl chains through covalent bonds to form an amphiphilic interface, hydrophilic polyethylene glycol chains enrich furfuryl alcohol molecules through hydrogen bonds, and hydrophobic alkyl chains capture hydrogen microbubbles, so that the gas-liquid interfacial tension can be effectively reduced, large bubbles can be broken, and nano bubbles can stably exist; and the preparation of tetrahydrofurfuryl alcohol realizes efficient reaction under obviously reduced pressure.

This scheme belongs to the field of organic synthesis technology, discloses the synthesis method of anticancer medicine darolutamide, and the synthesis method designs a new synthesis route: using formula (S1) compound as starting material, first converted into formula (1ab) or formula (1ac) compound, and then converted into formula (TM-1) compound; the obtained formula (TM-1) compound reacts with formula (1ad) or formula (1ae) compound converted from formula (S5) compound to synthesize formula (TM-2) compound, and then converted into formula (TM-3 compound); the obtained formula (TM-3) compound reacts with formula (S6) compound to synthesize formula (TM-4) compound, and then converted into formula (TM-5) darolutamide. The synthesis process does not need to use expensive palladium catalysts or ligands, so there is no problem of heavy metal residues or heavy metal toxicity in the drug product caused by palladium catalysts in the pharmaceutical process, and there is no need to remove trace metal residues from the target product; the raw materials used are cheap and easy to obtain, the reaction system is green and environmentally friendly, simple to handle, high yield, and good purity.

The application discloses an emulsion microreactor for cascade reaction and a preparation method and application thereof. The emulsion microreactor is prepared by the following steps: acidolysis of agar, hydrophobic modification, mixing of obtained interface stable modified agar nanoparticles, enzymes and buffer to obtain an aqueous phase; mixing of a substrate, a catalyst and an organic solvent to obtain an oil phase; and mixing of the aqueous phase and the oil phase to obtain the emulsion microreactor. The emulsion microreactor is used for synthesizing 4-biphenylcarboxylic acid ethyl ester by using lipase and a metal palladium catalyst, solves the problem of poor compatibility between the catalyst metal palladium and the lipase, spatially separates the lipase and the metal palladium, improves the cascade catalytic efficiency of the metal enzyme, and finally the yield of the product 4-biphenylcarboxylic acid ethyl ester can reach 55.85%; and the metal enzyme cascade reaction is completed in one pot in the emulsion microreactor, avoids separation of an intermediate product, expands the range of catalytic reactions, and provides a reaction platform for other high-value-added pharmaceutical intermediate products.

The invention belongs to the field of fine chemical engineering, and discloses a preparation method of halauxifen-methyl, which comprises the following steps: by taking a compound I and a compound II as raw materials and acetonitrile or an acetonitrile-water mixed solution as a reaction solvent, under the protection of nitrogen, taking a palladium catalyst as a catalyst and under the condition that a cocatalyst exists or does not exist, carrying out a reaction on the compound I and the compound II to obtain the halauxifen-methyl. And carrying out Suzuki coupling reaction on the compound I and the compound II to obtain the halauxifen-methyl. The method for preparing the halauxifen-methyl is high in novelty, the product selectivity can be improved by adding the cocatalyst, the product yield is high and at least reaches 80%, and the product purity is high. # imgabs0 #

Provided is an alkane production method wherein a continuous reaction of an alcohol and hydrogen proceeds at a low reaction pressure, carbon reduction from the alcohol can be suppressed, and the conversion rate is excellent. This alkane production method for producing an alkane from a C8-22 alcohol comprises a step in which the alcohol and hydrogen are continuously reacted under the following conditions. (i) The reaction is carried out in the presence of a zeolite carrier supporting palladium, the reaction temperature is 180°C or higher, and the hydrogen pressure is 0 MPa to 0.7 MPa in terms of gauge pressure. (ii) The space velocity (SV) of the hydrogen relative to the volume of a catalyst in which the palladium is supported on the zeolite carrier is 1200 h–1 to 2400 h–1. (iii) The space velocity (SV) of the alcohol relative to the volume of the catalyst in which the palladium is supported on the zeolite carrier is 8 h–1. (iv) The zeolite carrier is of an H-beta type or an H-ZSM-5 type, has a molar ratio (SiO2 / AL2O3) between silica (SiO2) and alumina (AL2O3) of 23 to 27, and has a palladium support quantity of 0.1 mass% to 5 mass%.

The invention provides a synthesis method of a thioether ligand and a palladium-catalyzed 2-aryl indole compound, and designs an application of the biphenyl thioether ligand and a palladium catalyst in preparation of the 2-aryl indole compound. Indole and arylboronic acid are subjected to a reaction under the action of a palladium catalyst and a biphenyl sulfide ligand, and the structural formula of the biphenyl sulfide ligand is shown in the specification. Ar is phenyl, furyl, thienyl, naphthyl or phenyl substituted by one or more substituent groups; r1 is methyl, methoxyl, fluorine atom, chlorine atom, bromine atom or methyl ester group; r2 is the same or different and is methyl, ethyl, isopropyl, isobutyl, cyclohexyl, benzyl, n-butyl or n-hexyl; r3 is alkoxy, alkylthio, substituted amino or halogen; the palladium catalyst is a divalent palladium compound.

The application discloses a crystalline hyperbranched multi-arm copolymer, a self-supporting graphene film and a preparation and application thereof. The crystalline hyperbranched multi-arm copolymer is prepared by the following method: a hyperbranched macromolecular initiator is obtained by using an alpha-diimine palladium catalyst to catalyze ethylene and a bromine-containing functional monomer in a one-step "chain removal" copolymerization in a water-free grade solvent; and then the hyperbranched macromolecular initiator is used to initiate atom transfer radical polymerization of an acrylate functional monomer to obtain the crystalline hyperbranched multi-arm copolymer. The crystalline hyperbranched multi-arm copolymer, graphite powder and a solvent are mixed in proportion, graphene initial dispersion liquid is obtained through ultrasonic and centrifugal separation, and then the self-supporting graphene film is obtained through filtration, elution and drying in sequence. The application provides an application of the self-supporting graphene film as an electrothermal film, and the self-supporting graphene film has excellent electrothermal performance and mechanical strength.

The application discloses a method for synthesizing organic acetylide ester through a palladium catalytic reaction and belongs to the field of organic synthesis. The organic acetylide ester is obtained through a cross-coupling reaction in the presence of a palladium catalyst, a phosphine ligand and an alkali, with terminal alkyne and di-tert-butyl dicarbonate as raw materials. The method has the advantages of high reaction yield, wide substrate range, good functional group compatibility, and the advantages of non-toxic and easy-to-obtain carbonyl source, simple operation steps and mild reaction conditions.

The application discloses a preparation method of a key intermediate of dapagliflozin, and belongs to the technical field of preparation of medical intermediates. The preparation method of the key intermediate of dapagliflozin comprises the following steps: 1, 1-ethoxy-4-methylbenzene is prepared by using p-cresol, sodium hydroxide and diethyl sulfate; 2, (4-ethoxybenzyl) phenyl sulfide is prepared by using 1-ethoxy-4-methylbenzene, thiophenol, a palladium catalyst, an alkali and an oxidant; 3, 1-benzyl-4-ethoxybenzene is prepared by using (4-ethoxybenzyl) phenyl sulfide under a hydrogen atmosphere; 4, 4-ethoxy-2'-chlorobenzhydrol is prepared by carrying out chlorination reaction on 1-benzyl-4-ethoxybenzene; and 5, 5-bromo-2-chloro-4'-ethoxybenzhydrol is prepared by carrying out bromination reaction on 4-ethoxy-2'-chlorobenzhydrol. The yield and purity of 5-bromo-2-chloro-4'-ethoxybenzhydrol prepared by the method are higher, the process is safer, and the production cost is reduced.

The application relates to the field of organic synthetic chemistry, in particular to a diamino diphosphine tetradentate ligand, a preparation method thereof and application of the diamino diphosphine tetradentate ligand in Suzuki cross-coupling reaction. The diamino diphosphine tetradentate ligand provided by the application has a structure shown in formula I; due to special spatial structure and electronic properties, the diamino diphosphine tetradentate ligand can provide multi-point coordination to metal and form a stable complex with the metal, so that the activity and stability of a palladium catalyst can be improved, the palladium catalyst can efficiently catalyze the Suzuki cross-coupling reaction for constructing a C-C bond at an extremely low dosage, and the diamino diphosphine tetradentate ligand and the metal palladium catalyst have strong universality to Suzuki cross-coupling reaction substrates, and have wide potential application value.

The invention discloses a method and a device for preparing a D-A type thermally activated delayed fluorescent material through continuous flow. A two-section type continuous flow reaction system is adopted, wherein the first continuous flow reaction system is connected with a tubular reactor in series through a micro-channel reactor, and efficient nucleophilic substitution reaction of an electron acceptor halide and an electron donor is achieved under palladium catalysis; the second continuous flow reaction system is driven by double feeding pumps, so that a D-A type compound prepared from a precursor and nonaphenyl tertiary alcohol are subjected to Friedel-Crafts alkylation modification under the catalysis of acid, the reaction time of the two steps is greatly shortened, and the yields of the two steps are both 88% or above. Through flow rate limitation, solvent concentration, solid content and temperature-pressure cooperative control, the problems of palladium-containing catalyst slurry transmission and side reaction inhibition are solved. According to the method, continuous kilogram-level production of the TADF material is achieved, compared with a traditional process, energy consumption is reduced, intermediate separation is not needed, and a new normal form is provided for industrial preparation of the OLED material.

The application belongs to the technical field of catalysts, and provides a titanium nickel nitride-based palladium catalyst, a preparation method and application thereof. The method comprises the following steps: mixing titanium tetrachloride, nickel acetate tetrahydrate and ethanol under an ammonia atmosphere, and performing a reaction to obtain a complex powder; performing a nitriding reaction on the complex powder under an ammonia atmosphere to obtain titanium nickel nitride nanoparticles; mixing the titanium nickel nitride nanoparticles, a chloropalladic acid solution, water and a potassium borohydride solution, and performing a reaction to obtain the titanium nickel nitride-based palladium catalyst. The catalyst prepared by the application has a high specific surface area and is composed of two parts, namely a titanium nickel nitride nanoparticle carrier and a supported Pd nanocluster. Among them, nickel atoms are doped between the titanium nitride crystal lattices. The Pd nanocluster is supported on the surface of the TiNiN carrier, and by adjusting the loading amount of Pd atoms, efficient and high-selectivity catalysis of various environmental hydrogenation catalytic processes can be realized.

The application discloses a preparation method of a phenylacetic acid compound, and particularly, the application uses a substituted or unsubstituted aromatic hydrocarbon as a starting material, and under the action of a palladium catalyst (such as palladium acetate, palladium on carbon, palladium chloride, tetra-triphenyl palladium, etc.), the starting material is reacted with formaldehyde, HCl (aq) and CO to efficiently generate the phenylacetic acid compound. The method disclosed by the application only needs to start from the aromatic hydrocarbon, greatly reduces the difficulty and cost of obtaining the raw material, and avoids stimulating, sensitizing or toxic raw materials. Compared with the prior art, the method disclosed by the application has the advantages of simplicity and efficiency, cheap and easy-to-obtain raw materials, high atomic economy, high yield, green and pollution-free, easy industrialization and the like.

The application belongs to the field of organic synthesis, and discloses a method for preparing chiral 2-(1,3-diarylallyl)malonate by using a Pd / phosphine oxygen bidentate phosphine phenol ligand catalysis, which comprises the following steps: under a protective atmosphere, mixing P, O-bidentate phosphine phenol ligand, a palladium catalyst, N, O-bis(trimethylsilyl)acetamide, a malonate nucleophilic reagent and an allyl acetate electrophilic reagent in dichloromethane, and reacting to obtain chiral 2-(1,3-diarylallyl)malonate product. The system has the advantages of high enantioselectivity, high catalytic efficiency, wide substrate application range and mild conditions.

A full continuous-flow preparation method of (+)-biotin, including: subjecting a cyclic anhydride and a chiral biphenyl propylene glycol to asymmetric ring-opening reaction to produce a first intermediate, which undergoes selective reduction with a borohydride and cyclization with an inorganic mineral acid to produce (3aS, 6aR)-lactone; subjecting the (3aS, 6aR)-lactone and a sulfenylating reagent to sulfenylation to produce (3aS, 6aR)-thiolactone, which undergoes Fukuyama coupling with a zinc reagent in the presence of a palladium catalyst and elimination reaction in the presence of an inorganic mineral acid to produce an alkenyl valerate compound; subjecting the alkenyl valerate compound to reduction in the presence of a Pd / C catalyst to produce a valerate ester, which undergoes hydrolysis to produce a valeric acid salt; and subjecting the valeric acid salt to debenzylation in the presence of an inorganic mineral acid to produce the target product (+)-biotin.

This invention discloses a magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd, its preparation method, and its applications. Using an amino alcohol as a starting material, an imidazole derivative containing a hydroxyl group on the N-substituent is obtained through a condensation and ring-closing reaction. This derivative is then subjected to substitution reactions with thionyl chloride and cyclohexanethiol sequentially to obtain an imidazole derivative containing a thioether on the N-substituent. This derivative is then reacted with 1,3-dibromopropane to obtain an N-bromopropyl-N'-cyclohexane thioether-substituted imidazole bromium salt. This salt is then reacted with Pd(OAc)₂ or PdCl₂ via a direct metallization reaction to obtain the N-bromopropyl-substituted thioether-chelated nitrogen heterocyclic carbene palladium complex NHC-Pd. The NHC-Pd complex is then reacted with amino-functionalized magnetic nanoparticles (MNPs-NH₂) to prepare the magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd. It not only possesses the activity of homogeneous nitrogen heterocyclic carbene palladium catalysts, but also has a simple synthesis method, high yield, and is easy to separate and reuse in catalytic C-C bonding reactions, showing good application prospects in the field of catalysis.

The invention discloses a gram-level synthesis method of Dactyllactone A. The gram-level synthesis method of Dactyllactone A is shown in the description. The method comprises the following steps: with simple and easily available aryl iodide, aziridine and triisopropyl silylacetylene as starting materials, stirring and reacting in an organic solvent at 60-70 DEG C under the action of a palladium catalyst, a phosphine ligand, a norbornene derivative and alkali to obtain a key intermediate; the key intermediate is condensed with iodo gem-dimethyl ester furanone prepared from propiolic acid and dimethyl malonate iodine ylide, and then the condensation product is subjected to an Au / Ag catalyzed intramolecular hydroamination reaction, photocatalytic 6-pi electro-cyclization and two-step conversion, so that the natural product Dactyllactone A can be obtained, wherein the iodo gem-dimethyl ester furanone and iodo gem-dimethyl ester furanone are prepared from propiolic acid and dimethyl malonate iodine ylide. The method has the advantages of cheap and easily available raw materials, short reaction steps, high reaction efficiency, large preparation scale, simple preparation process and the like, has great application potential, and lays a good foundation for industrial production.

The invention discloses a close-packed hexagonal-phase triangular-sheet-shaped nano-palladium catalyst and a preparation method thereof, and belongs to the technical field of nano-material preparation. According to the preparation method, palladium acetylacetonate is taken as a reactant, N, N-dimethylformamide is taken as a reaction solvent, hexadecyl trimethyl ammonium bromide is taken as a reducing agent and a crystal phase structure control agent, molybdenum hexacarbonyl is taken as a morphology control agent, and the close-packed hexagonal-phase triangular-sheet-shaped nano-palladium catalyst with regular morphology and controllable size is prepared through a simple liquid-phase thermochemical reduction method. The specific surface area of the two-dimensional sheet structure is large, the number of unsaturated atoms on the surface is large, interface charge transfer is fast, and improvement of the electro-catalytic performance is facilitated; and the triangular structure can provide more edge active sites, so that the catalytic activity can be further improved.

The invention provides a 1, 4-dihydrobenzosilacyclohexane compound containing a polyfunctional group structure as well as a preparation method and application thereof, the preparation method specifically comprises the following steps: in the presence of a phosphine ligand, a palladium catalyst and a reaction medium, carrying out silicon-carbon bond activation and cycloaddition reaction on phenylpropargyl aldehyde and benzosilacyclobutane to prepare the 1, 4-dihydrobenzosilacyclohexane compound containing the polyfunctional group structure, and carrying out cycloaddition reaction on the 1, 4-dihydrobenzosilacyclohexane compound containing the polyfunctional group structure to obtain the 1, 4-dihydrobenzosilacyclohexane compound containing the polyfunctional group structure. The 2, 4-dihydrobenzo-silacyclohexane compound disclosed by the invention is applied to both material chemistry and medicinal chemistry. According to the present invention, the reaction condition is mild, the operation is simple, the substrate universality is strong, the crude product is subjected to rapid column chromatography impurity removal and vacuum concentration to obtain the pure product, the post-treatment is convenient, the finally obtained chemical selection is high, and the silicon-containing cyclohexane structure precursor can be widely used in various organic reactions and drug synthesis, and has considerable potential application value.

This application discloses a negative curvature polycyclic aromatic hydrocarbon containing an eight-membered ring, its synthesis method, and its application, belonging to the field of organic synthesis. The synthesis method uses a haloacenaphthene derivative as a starting material. First, a tetrahalogenated key intermediate containing an eight-membered ring is constructed via a titanium tetrachloride-catalyzed cyclization tetramerization reaction. Subsequently, this intermediate undergoes a cyclization coupling reaction with an alkyne compound in the presence of a palladium catalyst, silver salt, and phosphine ligand to generate a negative curvature polycyclic aromatic hydrocarbon containing an eight-membered ring. The synthesis method of this application avoids multi-step precursor synthesis, resulting in a concise process. It allows for the flexible introduction of functional groups such as trifluoromethyl and silyl groups, improving the solubility and processability of the material. The obtained product exhibits a non-planar configuration, a narrow optical band gap, and excellent electron transport properties, making it suitable for applications... n Applications include semiconductors, chiral optoelectronic materials, and nano-carbon materials.

The invention relates to the technical field of biological medicine, in particular to a novel amino acid or polypeptide side chain carbonylation modification reagent which can be used as a novel carbonylation reagent in a method for synthesizing gamma-C (sp3)-H bond carbonylation amino acid or polypeptide through palladium catalysis. Substituting ethylene with a novel carbonylation reagent 1-iodine-2-bromine under the action of a palladium catalyst, an additive and a solvent to realize carbonylation and methylation of the amino acid gamma-C (sp3)-H bond. The method disclosed by the invention has the beneficial effects that a novel carbonylation reagent easy to prepare is developed, substrate raw materials are easy to obtain, the operation is simple and convenient, the condition is mild, the substrate application range is wide, and a plurality of carbonylated amino acids and polypeptide derivatives can be efficiently and accurately synthesized at low cost; and a novel method is provided for modification of unnatural amino acids and polypeptide side chains.

This invention belongs to the field of organic synthetic chemistry technology, specifically relating to a selenium-based indoloquinazoline derivative, its preparation method, and its application, comprising: in an organic solvent, using aromatic amine compounds, malononitrile, and diselenoether as raw materials, in the presence of a palladium catalyst and an organic base, at 90°C... o The reaction was carried out under C conditions with stirring to obtain a selenyl indoline quinazoline derivative. This method features mild reaction conditions, simple operation, high yield, and good functional group compatibility, conforming to the principles of green chemistry. Furthermore, the selenyl indoline quinazoline derivative provided by this invention exhibits good inhibitory activity against Plasmodium, providing a drug lead compound for the development of novel antimalarial drugs and holding significant importance for the prevention and / or treatment of malaria.

The utility model discloses an automatic hydrogenation nitrogen purification device, which relates to the field of purification devices, and comprises a rack, the top of the rack is fixedly connected with two dryers, a filter, a heater, two coolers, a deaerator and an electric cabinet, the two dryers are fixedly connected to the top of the rack, the two coolers are fixedly connected to the top of the rack, and the filter is fixedly connected to the top of the rack. And the two coolers are fixedly connected to the top of the rack. According to the automatic hydrogenation nitrogen purification device disclosed by the utility model, ordinary nitrogen enters the deaerator filled with the palladium catalyst deoxidation adsorbent, and a large amount of water generated under the action of the palladium catalyst deoxidation adsorbent after oxygen and hydrogen in the ordinary nitrogen are mixed is discharged, so that the residual oxygen content in the nitrogen can be less than ppm, and in view of saving energy consumption, the nitrogen purification efficiency is greatly improved. The adopted palladium catalyst deoxidizing adsorbent can achieve the deoxidizing effect without electric heating, the device does not need operators, all waste gas and waste water are discharged in a centralized mode, and sanitation and cleanliness of a plant are facilitated.

The application discloses a preparation method of baricitinib, and belongs to the technical field of drug synthesis. The method comprises the following steps: firstly, 2-[1-(ethylsulfonyl)-3-azetidinyl]acetonitrile and 4-pyrazole boron pinacol ester are subjected to a Michael addition reaction to obtain 1-(ethylsulfonyl)-3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl]-3-azetidine acetonitrile as an intermediate I; secondly, a protection group is introduced on the amino group of 4-chloropyrrolopyrimidine to obtain an intermediate II; finally, the intermediate I and the intermediate II are subjected to a Suzuki coupling process by adopting a method of combining a nickel pre-catalyst with a supporting ligand to obtain the baricitinib. The preparation method creatively realizes cross coupling of the baricitinib by adopting the cheap metal nickel as a catalyst, avoids the use of a heavy metal palladium catalyst, and has the advantages of low cost, low toxicity, small pollution, green environmental protection and the like.

The invention belongs to the field of organic synthesis, and particularly relates to a synthetic method of a diaryl methane compound. A toluene derivative as shown in a formula 1, an aryl iodide as shown in a formula 2 and a styrene derivative as shown in a formula 3 are subjected to a reaction in the presence of a catalytic amount of PdCl2 (dppf) and 4, 6-di (diphenylphosphine) phenazine and an equivalent amount of LiN (SiMe3) 2 and CsF to synthesize the diaryl methane compound as shown in a formula 4. The coupling reaction of the toluene derivative, the aryl iodide and the styrene derivative is realized by adopting a catalytic amount of PdCl2 (dppf), and the palladium catalyst shows obvious catalytic performance.