154results about "Magnesium organic compounds" patented technology

The invention relates to the technical field of preparation of small molecule compound medicines, in particular to a preparation method of (S)-flurbiprofen. The method comprises the following steps: dropwise adding a tetrahydrofuran solution of 4-bromo-2-fluorobiphenyl into a mixture of tetrahydrofuran and magnesium, and reacting to generate a Grignard reagent; mixing tetrahydrofuran, (S)-vinyl chloride oxide and ferric acetylacetonate, dropwise adding the Grignard reagent, performing acidolysis ring opening, and performing methylation with methyl iodide and magnesium iodide to obtain an alpha-hydroxyl aromatic carboxylic acid derivative; and reacting with sodium chlorite, nitroxide free radicals and acetonitrile, and oxidizing to obtain the (S)-flurbiprofen. By introducing a chiral induction unit, effective transmission of chiral information is realized in a coupling stage, an original chiral center is not destroyed in a subsequent reaction, and a product is ensured to have a highly consistent configuration. According to the scheme, the technical problem that a method capable of remarkably improving the optical purity and yield of (S)-flurbiprofen is lacked in the prior art can be solved, and the method has good environmental friendliness and industrial application prospects.

The invention discloses a method for preparing 3-phenanthrenol. The method comprises coupling a compound 3-tert-butoxyphenylboronic acid and o-bromobenzaldehyde to obtain 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, then reacting 2-(chloromethoxy)-2-methylpropane with magnesium chips in tetrahydrofuran to generate a Grignard reagent, followed by substitution with 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, and reflux and water separation with p-toluenesulfonic acid to obtain 3'-tert-butoxy-2-(2"-tert-butoxyvinyl)-1,1'-biphenyl, and finally ring closure with methanesulfonic acid and de-tert-butylation to obtain 3-phenanthrenol. The method introduces tert-butyl protection, thereby increasing steric hindrance and reducing isomers during ring closure, and facilitating deprotection conditions. The obtained product can have a purity of more than 99.0% without the need for column chromatography.

The present invention relates to a display device comprisinga plurality of OLED pixels comprising at least two OLED pixels, the OLED pixels comprising an anode, a cathode, and a stack of organic layers, wherein the stack of organic layersis arranged between and in contact with the cathode and the anode, andcomprises a first electron transport layer, a first hole transport layer, and a first light emitting layer provided between the first hole transport layer and the first electron transport layer, anda driving circuit configured to separately driving the pixels of the plurality of OLED pixels,wherein, for the plurality of OLED pixels, the first hole transport layer is provided in the stack of organic layers as a common hole transport layer shared by the plurality of OLED pixels, and the first hole transport layer comprises(i) at least one first hole transport matrix compound consisting of covalently bound atoms and(ii) at least one electrical p-dopant selected from metal salts and from electrically neutral metal complexes comprising a metal cation and at least one anion and / or at least one anionic ligand consisting of at least 4 covalently bound atoms,wherein the metal cation of the electrical p-dopant is selected from alkali metals; alkaline earth metals, Pb, Mn, Fe, Co, Ni, Zn, Cd; rare earth metals in oxidation state (II) or (III); Al, Ga, In; and from Sn, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W in oxidation state (IV) or less, a method for preparing the display device and a chemical compound for use therein.

The invention relates to a novel crystal form of serine magnesium represented by a chemical formula 1 and a preparation method thereof. The crystal form of the present invention has excellent thermal stability and moisture stability, can be stably stored without decomposition or crystal form transition even during long-term storage, and thus can be advantageously used as a pharmaceutical raw material for pharmaceutical products. # imgabs0 #

The present disclosure relates to a solid component for producing an olefin polymerization catalyst, its production method, and its use. The solid component contains (i) a magnesium compound represented by the following formula (1), (ii) a Lewis base (LB), and (iii) optionally a metal component other than magnesium, where LB is a compound represented by the general formula (II) or an amide compound represented by the general formula (II'). The solid component produced in the present invention has a good particle morphology, and a catalyst produced by using the solid component as a support is less likely to be crushed and has better stereostructure orientation in olefin polymerization, particularly propylene polymerization or copolymerization. [Formula 1] JPEG2023546624000060.jpg41169

To provide a production method for a phthalocyanine compound that enables high-purity production of a phthalocyanine compound having an ester side chain.SOLUTION: A method for producing a phthalocyanine compound comprises a step of mixing a phthalonitrile compound represented by general formula (1), a metal compound, and a compound represented by general formula (5), wherein in general formula (1), Z1 to Z4 each independently represent a hydrogen atom, a halogen atom, an alkoxy group, or the like, and at least one of Z1 to Z4 is a substituent represented by general formula (2); in general formula (2), L represents an alkylene or arylene group, and R represents an alkyl group or an aryl group; and in general formula (5), R is the same as R in general formula (2).SELECTED DRAWING: None

The present invention relates to a process for providing 4-chloro-2-(trifluoromethyl)phenyl Grignard compound. Further, the present invention relates to the process for preparation of 4-chloro-2-(trifluoromethyl)phenyl compounds from 4-chloro-2-(trifluoromethyl)phenyl Gri- gnard compound, in particular to the process for the preparation of substituted phenoxy- phenyl ketones.

Primary, secondary (1°,2°) alkylethylenediamine- and alkylpropylenediamine- appended variants of metal-organic framework are provided for CO2 capture applications. Increasing the size of the alkyl group on the secondary amine enhances the stability to diamine volatilization from the metal sites. Two-step adsorption / desorption profiles are overcome by minimizing steric interactions between adjacent ammonium carbamate chains. For instance, the isoreticularly expanded framework Mg2(dotpdc) (dotpdc4- =4,4"-dioxido-[1,1':4',l"-terphenyl]-3,3"-dicarboxylate), yields diamine-appended adsorbents displaying a single CO2 adsorption step. Further, use of the isomeric framework Mg-IRMOF-74-II or Mg2(pc-dobpdc) (pc-dobpdc4- = 3,3-dioxidobiphenyl-4,4-dicarboxylate, pc = para-carboxylate) also leads to a single CO2 adsorption step with bulky diamines. By relieving steric interactions between adjacent ammonium carbamate chains, these frameworks enable step-shaped CO2 adsorption, decreased water co-adsorption, and increased stability to diamine loss. Variants of Mg2(dotpdc) and Mg2(pc-dobpdc) functionalized with large diamines such as N-(n-heptyl)ethylenediamine have utility as adsorbents for carbon capture applications.

This invention relates to the field of organic synthesis technology, specifically to a highly efficient and stable Grignard preparation and its green preparation method. By weight, it comprises 8-18 parts of a magnesium source, 40-92 parts of a halogenated hydrocarbon, 150-200 parts of a green solvent, 15-20 parts of ethylene glycol dimethyl ether, and 2.3-3.2 parts of a synergistic stabilizer. The green solvent is 2-methyltetrahydrofuran, or a composite solvent with a weight ratio of 2-methyltetrahydrofuran:methyl tert-butyl ether of 150-160:40-50. The synergistic stabilizer is composed of 1.5-2.0 parts of N,N,N',N'-tetramethylethylenediamine and 0.8-1.2 parts of butylated hydroxytoluene, or composed of 1.5-2.0 parts of N,N,N',N'-tetramethylethylenediamine and 1.0 part of phenothiazine. This invention uses a green solvent system to replace traditional toxic and harmful solvents, and combines it with a solvent recovery process to achieve solvent recycling, which greatly reduces waste emissions and makes the production process safer and more environmentally friendly, in line with the development direction of green chemical industry.

The present invention discloses a method for preparing 1-aryl-3-arylsulfinylbicyclo[1.1.1]pentane. Under inert gas protection, an aryl Grignard reagent is reacted with [1.1.1] propeller alkane, and the resulting intermediate solution is reacted with an SO2 source. After the reaction is completed, 1-aryl-3-arylsulfinylbicyclo[1.1.1]pentane is obtained by post-processing. The present invention achieves efficient preparation of 1-aryl-3-arylsulfinylbicyclo[1.1.1]pentane without adding any catalyst, and has low raw material cost, easy operation, mild conditions, and high reaction yield, and has broad application value.

The invention provides a preparation method of pyruvic acid-1-13C, and relates to the technical field of chemical drugs, and the preparation method comprises the following steps: carrying out reaction and post-treatment on 13C-carbon dioxide and a Grignard reagent to obtain pyruvic acid-1-13C; wherein the Grignard reagent comprises a Grignard reagent obtained by reacting magnesium with acetyl halide. The technical problems that in the prior art, a pyruvic acid-1-13C synthesis method has safety risks, raw materials are not easy to obtain, the number of reaction reagent types is large, the number of process steps is large, and the yield is low are solved, the technical effects that safety and environmental protection are achieved, the raw materials are easy to obtain, the process is simple, and the synthesis route is short are achieved, and the obtained pyruvic acid-1-13C is high in purity and high in yield. And clinical test requirements can be met.

The invention relates to a method for synthesizing (R)-3-methylheptanoic acid. According to the method, the application range of steroid sapogenin degradation waste is further expanded. According to the method disclosed by the invention, the (R)-3-methyl-heptanoic acid can be conveniently obtained by taking the (R)-4-methyl-gamma-butyric acid lactone obtained by degrading steroid sapogenin as a raw material. According to the method provided by the invention, the use of highly toxic and controlled reagents is avoided, high-risk reactions such as hydrogenation in the prior art are avoided, and the method is mild in reaction condition and low in synthesis cost. Meanwhile, the utilization rate of steroid sapogenin resources is increased, and waste generated in the utilization process of the steroid sapogenin resources is reduced.

The present invention relates to halogenated alkenylalkoxymethyl ether compounds of the following general formula (1): R 1 CH2OCH2OCH2CH2CH=CH(CH2) a X 1 (1), wherein R 1 represents a hydrogen atom, a n-alkyl group having 1 to 9 carbon atoms, or a phenyl group, X 1 represents a halogen atom, and a represents an integer of 3 to 14. The present invention also relates to a method for producing terminal conjugated alkadien-1-yl acetate compounds of the following general formula (5): CH2=CHCH=CH(CH2) a OAc (5), wherein a is defined as above, and Ac represents an acetyl group, and a method for producing terminal conjugated alkadien-1-ol compounds of the following general formula (6): CH2=CHCH=CH(CH2) a OH (6), wherein a is defined as above.

The present invention relates to a process for the production of an intermediate useful in organic synthesis, in particular for the production of astaxanthin.

A process of manufacturing a functionalized porous material includes: mixing a base porous material comprising a porous structure and a labile ligand with a functionalizing agent to form a slurry, the porous structure having open metal sites and a plurality of pores, wherein the labile ligand is coordinated to the open metal sites, present in the plurality of pores but not coordinated to the open metal sites, or a combination thereof, the labile ligand has a first boiling temperature and the functionalizing agent has a second boiling temperature that is higher than the first boiling temperature; and drying the slurry to form a functionalized porous material comprising the functionalizing agent coordinated to the open metal sites.

The present invention provides 5-(2-butyl-1,3-dioxolan-2-yl)-1-methylpentyl acetate of the following formula (1). The present invention further provides the aforesaid 5-(2-butyl-1,3-dioxolan-2-yl)-1-methylpentyl acetate (1), the process comprising the step of subjecting an organic magnesium compound (2) of the following general formula (2), wherein X1 represents a halogen atom or a 3-(2-butyl-1,3-dioxolan-2-yl)propyl group, to a nucleophilic addition reaction with propylene oxide of the following formula (3) and then reacting with an acetylating agent of the following general formula (4), wherein X2 represents a halogen atom, an acetoxy group, a methoxy group, or an ethoxy group, to form 5-(2-butyl-1,3-dioxolan-2-yl)-1-methylpentyl acetate (1).

Provided is a metal hydroxide composite including a base layer, a surface layer, and an active ingredient, the metal hydroxide composite including a multilayer hydroxide structure of Chemical Formula 1; a metal hydroxide composite prepared by including a step of co-precipitating an active ingredient and a metal hydroxide structure precursor by a precipitation reaction using an alcohol and water, and a method for preparing the same.

To provide a metal complex which is useful for producing a negative electrode active material having superior initial coulombic efficiency and capacity retention and a method for producing the same, a negative electrode active material precursor containing the metal complex and a method for producing the same, a negative electrode active material, and a secondary battery having the negative electrode active material.SOLUTION: A metal complex contains a metal cation, the counterion of which includes a carboxylate anion having 2-20 carbon atoms and having a protected amino group.SELECTED DRAWING: None

The method discloses a green synthesis process of acetylene alcohol double Grignard reagent, and the synthesis process comprises the following steps: dissolving benzyl chloride in an organic solvent to prepare solution A, adding metal magnesium to solution A to initiate a reaction, and preparing an initiation reaction solution; (2) dissolving benzyl chloride and acetylene alcohol substances in an organic solvent to prepare solution B; (2) adding solution B in step (2) to the initiation reaction solution in step (1) dropwise to perform a reaction, and preparing acetylene alcohol double Grignard reagent. The application provides a new synthesis method for synthesizing acetylene alcohol double Grignard reagent by using benzyl magnesium chloride, which can avoid a coupling side reaction between benzyl Grignard reagent and benzyl chloride, and does not need excessive metal magnesium.

The present invention relates to an organic electronic device comprising a semiconductor layer, wherein the semiconductor layer comprises a compound of formula (1).

The present disclosure provides a composite metal salt having a hexagonal Cd(OH)2 type crystal structure and an X-ray diffraction intensity ratio (orientation H) of the (101) plane to the (001) plane of 60% or less, and being denoted by the following formula (1):wherein “M2+” denotes at least one divalent metal other than Mg; “A” denotes at least one organic ligand; “x” denotes a number in a range of 0≤x<0.2; “y” denotes a number in a range of 0<y<0.05; and “n” denotes an integer of from 1 to 4, or zero.

The invention provides a method for efficiently preparing L-menthyl formic acid. The method comprises the following steps: a) dispersing magnesium chips, an initiator and anhydrous lithium halide in an ether organic solvent; b) dropwise adding 10% of L-menthyl chloride required by reaction into the previous step, then heating to a corresponding initiation temperature, then continuously dropwise adding the rest L-menthyl chloride, and carrying out heat preservation and stirring after dropwise adding is finished; and c) introducing carbon dioxide gas into the solution obtained in the previous step, and then adding acid for quenching reaction to obtain a target product. According to the method, L-menthyl chloride, magnesium chips and carbon dioxide are used as reaction raw materials, alkyl magnesium chloride is used as an initiator, and anhydrous lithium halide is used as a stabilizer, so that the stability of L-menthyl magnesium chloride is improved, and high-purity L-menthyl formic acid is obtained at a relatively high yield in the reaction process.

A method for producing a metal-organic framework (MOF) compound comprising a MOF metal and a MOF linker is disclosed. The method includes forming a mixture comprising a MOF metal precursor, a MOF linker precursor, a solvent, and optionally a base. The method also includes reacting the mixture under reaction conditions selected from the group consisting of ambient reaction pressure, a mixture temperature below about the boiling point of the solvent, an aqueous reaction mixture, and combinations thereof. The MOF compound produced by the method is also disclosed.

The present invention provides a (6Z)-6-tridecenyl metal compound (1) wherein M1 represents Li or MgZ1, and Z1 represents a halogen atom or a (6Z)-6-tridecenyl group; also provided is a method for preparing a compound (1) comprising the steps of: preparing a (3Z)-3-decenyl metal compound (3) from a 1-halo-(3Z)-3-decenyl compound (2), where X1 represents a halogen atom, where M2 represents Li or MgZ2, and Z2 represents a halogen atom or a (3Z)-3-decenyl group; a coupling reaction of the compound (3) with a 1, 3-dihalopropane compound (4), where X2 and X3 independently of each other represent a halogen atom, to form a 1-halo-(6Z)-6-tridecene compound (5), where X4 represents a halogen atom; and preparing a (6Z)-6-tridecenyl metal compound (1) from the compound (5).

To provide a method for preparing an in situ metal doped manganese iron oxalate precursor.SOLUTION: Iron source, manganese source, doped metal elements (Mg, Zn, etc.) are weighed according to a stoichiometric ratio, and deionized water is added to the weighed metal to ultrasonically dissolve the weighed metal to obtain a mixed metal solution. The mixed metal solution is added to a prepared oxalic acid solution and subsequently a certain concentration of complexing agent is added to the solution to perform co-precipitation reaction under the protection of inert gas. A resultant suspension of metal doped manganese iron oxalate is recovered and then filtered, washed and dried to obtain a powder of manganese iron oxalate precursor.EFFECT: By using the manganese iron oxalate precursor as the iron and manganese sources, this can effectively avoid the problem of uneven mixing due to the iron and manganese sources. Moreover, lithium manganese iron phosphate synthesized from the manganese iron oxalate precursor after metal doping can significantly improve the electronic conductivity, thereby enhancing the electrochemical properties of lithium manganese iron phosphate.SELECTED DRAWING: Figure 1

The present application relates to an intermediate of fulvestrant and a preparation method thereof. Specifically, the present application relates to a compound as shown in formula V and a preparation method thereof, wherein R 1 is hydrogen or a hydroxyl protecting group. The present application also relates to a preparation method for synthesizing fulvestrant via the compound as shown in formula V, which has the advantages of short reaction steps, mild and safe reaction conditions, high selectivity, simple operation and purification, high synthesis efficiency, and is suitable for large-scale production.

The application discloses a kind of organic metal catalyst based on biguanide-based ligand and its preparation method and application, belong to polymer material field.The organic metal catalyst is by the ligand with biguanide-based structure and magnesium salt coordination and form.The preparation method of the application is simple, condition is mild, the obtained organic metal catalyst is with magnesium as metal center, its toxicity is lower, catalytic activity is high, can successfully catalyze cyclic lactone under solvent or solvent-free condition ring-opening polymerization reaction, and product molecular weight is high, distribution is narrow.

The application discloses a rare earth nitride-containing aminomagnesium-lithium hydride composite hydrogen storage material and a preparation method thereof. The rare earth nitride-containing aminomagnesium-lithium hydride composite hydrogen storage material comprises a rare earth nitride and an aminomagnesium-lithium hydride composite system. The preparation method comprises the following steps: mixing aminomagnesium with lithium hydride, adding the rare earth nitride in the mixing process, transferring the mixed mixture into a ball mill tank, and ball milling under inert gas protection to obtain the rare earth nitride-containing aminomagnesium-lithium hydride composite hydrogen storage material. The raw material synthesis process is simple and controllable, and the cost is low. The hydrogen storage performance of the aminomagnesium-lithium hydride composite hydrogen storage material can be obviously improved by adding a small amount of the rare earth nitride. Moreover, the rare earth nitride can be purchased through a commercial channel, and the adding mode can be directly mixed with the raw material.

The purpose of the present disclosure is to provide magnesium glycinate which has a high magnesium concentration.　Disclosed is magnesium glycinate which is configured such that, in differential scanning calorimetry analysis, the value S1 / S2 obtained by dividing the area S1 of an endothermic peak that has a starting temperature in the range of 230°C to 255°C by the area S2 of an endothermic peak that has a starting temperature in the range of 330°C to 370°C is 0 to 7 inclusive.

The invention discloses a continuous flow preparation method and a preparation system of a Grignard reagent, and belongs to the technical field of Grignard reagent preparation. The method comprises the following steps: filling magnesium particles with the particle size of 1-10mm in a micro-channel tubular reactor; a halogenated hydrocarbon solution is introduced from the bottom of the microchannel tubular reactor, the Grignard reagent flows out from the top of the microchannel tubular reactor, the retention time of the reaction is 10-45 min, and after the reaction is completed, the Grignard reagent with proper concentration is directly obtained without separating magnesium; the micro-channel tubular reactor is vertically arranged, and filter screens are arranged on a feed port in the bottom and a reaction liquid discharge port in the top of the micro-channel tubular reactor; the magnesium particles are supplemented from the top of the micro-channel tubular reactor. Compared with the prior art, efficiency and safety can be remarkably improved.