190 results about "Heck reaction" patented technology

The invention discloses visual, portable and quick mercury ion detection test paper and a preparation method and application thereof. The preparation method of the test paper comprises the following steps: firstly preparing rhodamine hydrazide, carrying out etherification and Heck reaction on hydroxyl on filter paper so as to introduce in required isosulfocyanate radical end group, grafting the prepared rhodamine hydrazide onto the filter paper to finally obtain the mercury ion detection test paper. The prepared detection test paper has the advantages that a rhodamine derivative fluorescence probe and the filter paper are chemically bonded, the structure is firm, the reaction speed is high, the detection limit is 10mu m, the selectivity is good, the influences from other various coexisting ions are avoided, the detection environment is an organic-solution-free total aqueous solution system containing mercury ions, the pollution of other organic solvents to the environment is reduced; and under the irradiation of an ultraviolet lamp, the test paper can realize visual detection; the detection measures are convenient and can be performed on site; and therefore, the test paper and the preparation method of the test paper have great application prospect in the field of water pollution caused by mercury ions.

The invention discloses a chitosan-based porous microsphere load palladium catalyst, a preparation method and application thereof, belonging to the technical field of chemical catalyst preparation technology. The catalyst is characterized in that a catalyst carrier is a chitosan-based porous microsphere of which the diameter is 0.5-3 mm, the aperture of the surface is 5-30 nm, and the internal aperture is 1-10 mu m; an active component is palladium which accounts for 1-5 wt% of the carrier. The chitosan-based porous microsphere load palladium catalyst is applied to catalysis Ullmann and Heck reaction, can greatly reduce operation steps, material consumption and the like in the industrial production of Ullmann and Heck reaction, is favourable for lowering production cost and is environmental friendly.

Chiral ligands and transition metal complexes based on such chiral ligands useful in asymmetric catalysis are disclosed. The chiral ligands include phospholanes, P,N ligands, N,N ligands, biphenols, and chelating phosphines. The ferrocene-based irridium (R,R)-f-binaphane complex reduces imines to the corresponding amines with 95-99.6% enantioselectivity and reduces beta-substituted-alpha-arylenamides with 95% enantioselectivity. The transition metal complexes of the chiral ligands are useful in asymmetric reactions such as asymmetric hydrogenation of imines, asymmetric hydride transfer reactions, hydrosilylation, hydroboration, hydrovinylation, hydroformylation, allylic alkylation, cyclopropanation, Diels-Alder reaction, Heck reaction, isomerization, Aldol reaction, Michael addition and epoxidation reactions.

A process for producing cinnamic acids and alkyl esters thereof, particularly, fluorinated cinnamic acids and alkyl esters thereof. The process comprises reacting the appropriate bromobenzene and acrylic acid ester in a palladium-catalyzed HECK reaction under JEFFREY conditions using a phase-transfer catalyst (PTC) and an organic base to produce the corresponding cinnamic acid ester, and then preferably hydrolyzing the resulting ester under appropriate basic conditions, e.g. in the presence of a hydroxide, and precipitating the corresponding cinnamic acid product.

The invention discloses a sinomenine derivative and a synthesis method and aapplications thereof, wherein halogen, carbon-carbon double bond substituent and isoxazoline heterocyclic ring substituent are introduced to the 1-site of the sinomenine ring A. When the sinomenine derivative is prepared, sinomenine is used as the matrix and the synthesis technology containing microfluidic synthesis is adopted to perform Heck reaction and 1,3-dipolar cycloaddition reaction on the 1-site of sinomenine and generate the sinomenine derivative. The obtained compound has better anti-inflammatory activity and is potential to be used for curing arthritis and rheumatoid arthritis and used in the anti-inflammatory medicines thereof.

The invention relates to a kind of supported bimetallic complex catalyst of arylation to alkene by aryl halogenide and its preparing method. The catalyst contains precious metal Pd and/or base metal Cu, or Mo, or Ni, or Co, or Mn and carrier; the weight ratio of content of precious metal Pd counted as Pd and added carrier is 0.1% - 2.0%; the ratio of content of base metal counted as metal and added carrier is 0.5% - 10%. On the basis of precious metal Pd, add the other base metal Cu, or Mo, or Ni, or Co, or Mn; using chemical reduction method, prepare supported bimetallic complex catalyst used in Heck reaction; the watery solution concentration of reducing agent is 0.5% - 10%. The invention has following advantages: it has high catalyzing activeness, and short reacting time; it reduces the Pd dosage, and is easy to realize separation of output and catalyst.

The invention discloses gemini ionic liquid with fluorous biphasic property. The molecular formula of the ionic liquid is [(R1N2C3H3)2R]2+.[2X-]. The structure of the ionic liquid is shown as the general formula (I) in the specification, wherein R1 represents hydrogen or C1-C8 alkyl; R represents ethylidene oxyl element, is selected from-(CH2CH2O)qCH2CH2- and is formed by polyethylene glycol 400-10000, and q is 6-250; and X represents HBF4, HPF6, HNO3 or halogenated hydrogen. A catalyst can be prepared immediately after adding palladium, rhodium or nickel catalyst into the gemini ionic liquid with fluorous biphasic property for coordination, and can be used in HECK reaction, C-C coupling reaction and isomerization reaction. The ionic liquid is not easy to volatilize, and the catalyst prepared by utilizing the ionic liquid is used in HECK reaction, C-C coupling reaction and isomerization reaction, has high catalytic efficiency and can be reused.

The invention discloses a method for preparing 6-hydroxy-2(1H)-quinolone in ionic liquid by using a one-pot method. The invention synthesizes the 6-hydroxy-2(1H)-quinolone by through bromination, acidation and intramolecular Heck reaction of p-methoxy aniline and acryloyl chloride as raw materials in the ionic liquid by using the one-pot method. The method has simple synthesis line, low product cost and high yield, is environmental friendly and is easy to realize industrial production.

The invention relates to a preparation method for Palbociclib. The method comprises the following steps: taking 4-[6-(6-bromo-8-cyclopentyl-5-methyl-7-oxo-7,8-dihydro-pyridino[2,3-d]pyridine-2-yl-amino)-pyridine-3-yl]-piperazine-1-carboxylic acid tert-butyl ester as a starting raw material; performing Heck reaction, rearrangement, deprotection and neutral reaction to obtain the Palbociclib, wherein the total yield is 70 to 80 percent. According to the preparation method disclosed by the invention, non-Pd-catalyzed heck reaction is investigated, such that a phosphorus-containing ligand which is high in cost and needs harsh reaction conditions is avoided, and the production cost and the technological operation risk are reduced; acetylchloride is used for rearrangement and deprotection reaction to obtain Palbociclib hydrochloride, and the Palbociclib hydrochloride is alkalized to obtain the high-purity Palbociclib.

The invention belongs to the technical field of preparation of supported nano crystal catalysts and in particular relates to in situ controllable equipment for hydrotalcite-supported Pd nano crystal catalysts with different morphologies and research on activity of the hydrotalcite-supported Pd nano crystal catalysts in catalysis of a Heck coupled reaction. The synthesis process of the hydrotalcite-supported Pd nano crystal catalyst comprises the following step of: growing Pd nano crystals with different morphologies (cube, truncated octahedron and triangle) and different exposed crystal faces ({111} and {100}) in situ on the surface of hydrotalcite by adopting a one-pot synthesis method under the conditions of different reducing agents (polyvinylpyrrolidone and ethylene glycol) and surface capping agents (I<->, Cl<-> and polyvinylpyrrolidone) with a mixed solution composed of Na2PdCl4 and nitrate intercalation hydrotalcite. Besides, the synthesized hydrotalcite-supported Pd nano crystal catalysts with different morphologies are used for evaluating the Heck coupled reaction and researching a catalytic activity sequence of different exposed Pd crystal faces of the hydrotalcite-supported Pd nano crystal catalysts, and a foundation is laid for further reasonably designing an efficient supported nano crystal catalyst.

The invention discloses a novel synthesis method of a polyfluorene derivative and an application in a flow injection fluorescent sensor for a tumor marker. The synthesis method of the polyfluorene derivative comprises the following steps that: 1,4-dibromo p-phenylenediamine (a compound 1) is synthesized; 2,7-dibromo-9,9-bi(3'-(N,N'-dimethylamino) propyl)-fluorene (a compound 2) is synthesized; p-vinyltoluene (a compound 3) is synthesized; the three monomers are polymerized into the polyfluorene derivative by a Heck reaction. A fabrication method of the sensor comprises the following steps that polymethyl methacrylate is adopted to fabricate a flow injection fluorescent flow cell; ferroferric oxide magnetic particles and gold nanoparticles are prepared and assembled into gold covered ferroferric oxide; a primary antibody is modified on gold cladded ferroferric oxide; the polyfluorene derivative is subjected to silicon cladding treatment; a secondary antibody is modified on the surface of the silicon cladded polyfluorene derivative; an immune reaction is conducted; and flow injection fluoroscopic detection is conducted on the tumor marker. The sensor is strong in specificity, high in sensitivity, simple to operate, and low in detecting line.

The invention relates to a recoverable ligand-free mesoporous polymer palladium catalyst and a synthetic method and application thereof. The catalyst has a two-dimensional hexagonal ordered mesostructure. specific surface area is 250-380 m<2>/g; pore diameter is 3.0-7.0 nm; mass content of a functional phase transfer agent is 8.5-13 wt%; mass content of metal palladium is 1-5 wt%; and particle size of palladium particles is 3-5 nm. The preparation comprises the following steps: adding a surfactant and hydrochloric acid into an organic solvent, stirring and reacting, successively adding a silicon source, quaternary ammonium salt and a carbon source, continuously stirring and reacting; carrying out a thermosetting reaction, and then carrying out high-temperature calcining to prepare a functional mesoporous polymer carrier; and mixing the functional mesoporous polymer carrier and a palladium source, stirring, carrying out suction filtration, washing, carrying out vacuum drying, and carrying out a reduction reaction. The catalyst is applied in aqueous medium catalysis of a Heck reaction between bromobenzene and styrene for generation of stilbene. In comparison with the prior art, the method of the invention is simple; and the catalyst is efficient and stable, can be recycled for many times and has a wide application prospect in the field of industrial catalysis.

The invention provides a Pd complex catalyst as well as a preparation method and application thereof. The Pd metal complex catalyst provided by the invention has the structure shown by a formula (I), wherein R1 and R2 are alkyls or halogens; preferably, R1 is alkyl with 1-15 carbons, and R2 is alkyl with 1-5 carbons, or halogen; more preferably, R1 is methyl, ethyl, propyl or benzhydryl, and R2 is methyl or chlorine. DBCPh-NH2 is 2,6-bi (diphenylmethyl)-4-chloroaniline. According to the Pd metal complex catalyst, Heck reaction can be promoted when less Pd metal complex catalyst is used; and furthermore, the Pd metal complex catalyst has good catalytic performance and can be used for realizing the catalysis for the Heck reaction.

The invention relates to a preparation method of recessive malachite green hapten. The preparation method adopts the Heck reaction to lengthen an active arm, is mild in reaction conditions, adopts a small quantity of organic solvent, generates a small quantity of reaction byproducts and adopts simple operation steps; moreover, by optimizing a method for purifying the product, a great quantity of organic solvent is avoided being used in the purifying process and emission of environmental pollutants is effectively reduced.

The invention provides a Pd complex catalyst as well as a preparation method and application thereof. The structural formula of the Pd metal complex catalyst provided by the invention is shown in the formula II (shown in the description), wherein R1 and R are H and alkyl groups; preferably, R is a methyl or ethyl, and R1 is H or the methyl. According to the invention, a small amount of the Pd metal complex catalyst can be used to promote the Heck reaction, has an excellent catalytic performance and can catalyze the Heck reaction, and the formula I is also shown in the description.

Chiral ligands and metal complexes based on such chiral ligands useful in asymmetric catalysis are disclosed. The metal complexes according to the present invention are useful as catalysts in asymmetric reactions, such as, hydrogenation, hydride transfer, allylic alkylation, hydrosilylation, hydroboration, hydrovinylation, hydroformylation, olefin metathesis, hydrocarboxylation, isomerization, cyclopropanation, Diels-Alder reaction, Heck reaction, isomerization, Aldol reaction, Michael addition; epoxidation, kinetic resolution and [m+n] cycloaddition. Processes for the preparation of the ligands are also described.

The invention provides a preparation method of a compound III. The preparation method is characterized in that diacyl peroxide I and a compound II containing carbon-carbon double bonds are subjected to a coupling reaction in the presence of catalysts to produce the compound III. The diacyl peroxide is introduced into a Heck reaction as an efficient and controllable alkylating agent for the first time in the method, and the method has the advantages that raw materials and catalysts are cheap, the reaction condition is mild, the operation is simple, the reaction is efficient and the like.