78 results about "Magnesium bromide" patented technology

The invention discloses desulfurized rubber modified asphalt and a preparation method thereof, and the desulfurized rubber modified asphalt comprises the following components in parts by mass: 100 parts of petroleum asphalt, 25-35 parts of desulfurized rubber powder, 0.2-2 parts of oxime sulfonate modifier, and 0.5-3 parts of modified artificial zeolite. Wherein the desulfurized rubber powder is prepared from the following raw materials: waste rubber powder, calcium nitrate, aniline, 2, 5-benzothiazole dithiol, p-methylphenyl magnesium bromide, diphenyl sulfoxide and trimethylchlorosilane in a mass ratio of (80-100): (10-20): (20-30): (5-10): (5-6): 1: (3-4); the invention further discloses a specific preparation method of the desulfurized rubber powder. The asphalt provided by the invention has the advantages of simple components, improved performances, low mixing temperature and more convenient use.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of perfluorohexyl octane. The preparation method comprises the following steps: by taking perfluorohexyl ethyl iodide as a raw material, firstly carrying out Grignard reagent exchange with a reagent A, and then carrying out nucleophilic addition reaction with n-hexanal to obtain a compound III; carrying out esterification and substitution on the compound III to prepare a compound V, or carrying out an Apple substitution reaction to prepare the compound V; and carrying out reduction reaction on the compound V, rectifying and purifying to obtain a target product. The reagent A comprises an isopropyl magnesium chloride tetrahydrofuran solution, a methyl magnesium chloride tetrahydrofuran solution, a methyl magnesium bromide tetrahydrofuran solution, an ethyl magnesium chloride tetrahydrofuran solution, an ethyl magnesium bromide tetrahydrofuran solution and / or a phenyl magnesium bromide tetrahydrofuran solution. According to the method, the perfluorohexyl ethyl iodide and the n-hexanal are used as raw materials to prepare the perfluorohexyl octane, isomer impurities are fundamentally avoided, and the method has the advantages that purification is easy, the yield is high, the product purity is high, and industrial production is facilitated.

A phase change material composition for latent heat storage is provided. The composition includes a eutectic mixture of two or more salt hydrates, and at least one salt additive each selected from a bromide salt and a bromide salt hydrate. The mixture of salt hydrates has a melting temperature above room temperature. The at least one salt additive decreases the melting temperature of the mixture and reduces a degree of supercooling of the mixture. The mixture of salt hydrates may be a mixture of calcium chloride hexahydrate and magnesium chloride hexahydrate. The salt additives may include both calcium bromide and magnesium bromide. The melting temperature of the phase change material composition may be in a range of approximately 15 to 25° C. A thermal energy storage system including the phase change material composition and a method of heat management in the thermal energy storage system are also provided.

The invention discloses a preparation method of 2, 2, 4-trimethyl-1, 2-dihydroquinoline, and relates to a preparation method of 2, 2, 4-trimethyl-1, 2-dihydroquinoline. The method comprises the following steps: by taking o-aminoacetophenone and isobutenyl magnesium bromide as raw materials, reacting in the presence of a polymerization inhibitor and a solvent, then adding water to decompose, extracting, distilling to remove the solvent and lightly separating to obtain high-purity and high-yield 2, 2, 4-trimethyl-1, 2-dihydroquinoline. By adopting the method, carcinogenic primary amine impurities are not generated.

This invention relates to the field of magnesium primary battery preparation technology, and discloses a magnesium aqueous primary battery system, including a positive electrode, a negative electrode, and an electrolyte. The negative electrode is any one of magnesium metal and magnesium alloy. The positive electrode is made of a positive electrode active material, superconducting carbon, and a first-order gelatinizing agent. The electrolyte is made of magnesium bromide, a corrosion inhibitor, and a second-order gelatinizing agent. The preparation method includes the following steps: S1: preparing a positive electrode slurry; S2: preparing an electrolyte by introducing a corrosion inhibitor into the magnesium bromide electrolyte, followed by adding a second-order gelatinizing agent for gelatinization treatment to obtain a slow-release gelatinized electrolyte; S3: preparing a positive electrode steel shell; S4: assembling the battery. The technical solution of this invention not only slows down the corrosion rate of the negative electrode material and improves the utilization rate of the negative electrode material, but also solves the problems of voltage hysteresis and volume expansion during battery discharge; furthermore, it can match the reaction rates of the positive and negative electrodes.

The invention provides a preparation method of a natural product 6-HHS. The method comprises the following steps: reacting a compound 1 sanguinarine with vinyl magnesium bromide to prepare a compound 2; and reacting the compound 2 with a borane tetrahydrofuran complex to prepare 6-HHS. According to the method, sanguinarine is used as a raw material to prepare the natural product 6-HHS, the synthesis route is short, the synthesis efficiency is high, the yield of each step is 85% or above, the comprehensive yield of the natural product 6-HHS can reach 76%, operation is easy and convenient, the purity is high, and a simple, convenient and efficient way can be provided for chemical synthesis of 6-HHS.

The invention discloses a preparation method of 4-chloro-2-fluoro-3-methoxyphenylboronic acid and a preparation method of the 4-chloro-2-fluoro-3-methoxyphenylboronic acid. The specific implementation process comprises the following steps: by taking 1-bromo-4-chloro-2-fluoro-3-methoxybenzene as a raw material, carrying out Grignard reaction on magnesium chips and an initiator in an organic solvent to synthesize 4-chloro-2-fluoro-3-methoxyphenyl magnesium bromide; and the 4-chloro-2-fluoro-3-methoxyphenyl magnesium bromide and boric acid ester are synthesized into the 4-chloro-2-fluoro-3-methoxyphenylboronic acid, and then the 4-chloro-2-fluoro-3-methoxyphenyl magnesium bromide and boric acid ester are synthesized into the 4-chloro-2-fluoro-3-methoxyphenylboronic acid. The novel synthesis method of 4-chloro-2-fluoro-3-methoxyphenylboronic acid is designed, the total synthesis yield of the method ranges from 88% to 95%, compared with an existing synthesis route, the problems that a traditional route relates to an ultralow temperature condition and strong alkali, is low in safety and high in cost are solved, and the method has the advantages of being simple, environmentally friendly, safe, efficient and the like and is suitable for industrial production. Meanwhile, the method has a relatively good industrialization prospect.

The application discloses a kind of bromine iodine lead cesium perovskite solar cells of doping magnesium bromide prepared in low humidity environment and preparation method thereof, belong to perovskite photovoltaic technical field, including ITO transparent conductive glass and sequentially coated on ITO transparent conductive glass dense layer TiO2, SnO2 layer, bromine iodine lead cesium perovskite light-absorbing layer of doping magnesium bromide, 2,2',7,7'-tetra [N,N-di (4-methoxyphenyl) amino] -9,9'-spirobifluorene hole transport layer of doping lithium salt, silver electrode, and its preparation method is disclosed, the application is by doping into bromine iodine lead cesium perovskite precursor doping different molar magnesium bromide to optimize the energy level matching between perovskite and electron transport layer and hole transport layer, effectively reduce the recombination probability of carrier and improve the mobility of carrier, improve the crystal quality of perovskite thin film, to realize the light absorption coefficient of optimization light-absorbing layer, finally realize the improvement of bromine iodine lead cesium inorganic perovskite solar cell photoelectric conversion efficiency.

The invention relates to the technical field of medical and chemical medicines, in particular to a novel synthesis method of L (-)-threo-3-hydroxyaspartic acid hydrochloride. The preparation method comprises the following steps: by taking cheap and easily available D-phenylglycinol as an initial raw material, firstly protecting amino with Boc anhydride, then oxidizing to obtain N-BOC-D-phenylalanine aldehyde 3, then carrying out Grignard reaction on the N-BOC-D-phenylalanine aldehyde 3 and vinyl magnesium bromide at low temperature to obtain corresponding o-amino alcohol, then reacting the o-amino alcohol with 2, 2-dimethoxypropane at 0 DEG C under the catalytic action of p-toluenesulfonic acid, and finally obtaining the 2, 2-dimethoxypropane. The obtained compound 4 is subjected to Upjohn dihydroxylation reaction and sodium periodate oxidation to obtain corresponding aldehyde, and then the aldehyde is oxidized by potassium permanganate under a weak acidic condition to obtain corresponding carboxylic acid 5. Oxidizing a benzene ring by taking ruthenium trichloride as a catalyst and sodium periodate as a co-oxidant to obtain dicarboxylic acid; and finally, refluxing and deprotecting by using hydrochloric acid to obtain the L (-)-chloro-3-hydroxyaspartic acid hydrochloride.

The invention relates to a synthesis method of chiral N-Fmoc-2-methyl azetidine-2-carboxylic acid, and relates to the technical field of organic synthesis.The synthesis method comprises the following steps that Fmoc-alpha-methyl-L-glutamic acid-5-tert-butyl ester is subjected to deprotection, and a compound I is obtained; carrying out esterification reaction on the compound I and aryl halide in an alkaline solution to obtain a compound II; removing an Fmoc protecting group from the compound II in an alkaline solution to obtain a compound III; the compound III is subjected to lactamization under the action of trimethylchlorosilane and tert-butyl magnesium bromide, and a compound IV is obtained; selectively reducing amide of the compound IV under the action of a borane reducing reagent to obtain a compound V; hydrolyzing the compound V in an alkaline solution, and removing benzyl to obtain a compound VI; and protecting the amino group of the compound VI through Fmoc to obtain a compound VII, namely the chiral N-Fmoc-2-methyl azetidine-2-carboxylic acid. The method has the effect of improving the synthesis efficiency of the chiral N-Fmoc-2-methyl azetidine-2-carboxylic acid, and the product has high yield and purity.

The invention discloses a polysubstituted cyclopropyl carbonyl compound with calcium ion channel regulation activity as well as a pharmaceutical composition and application thereof, and belongs to the technical field of medicines. An alpha-chlorocyclobutanone compound is used as a raw material and reacts with aryl magnesium bromide with different substituent groups in an organic solvent, and the polysubstituted cyclopropyl carbonyl compound is obtained in one step. The polysubstituted cyclopropyl carbonyl compound is novel in structure, the preparation method has the advantages of being low in cost, simple and convenient to operate, mild in condition and the like, and the polysubstituted cyclopropyl carbonyl compound novel in structure can be rapidly obtained. The prepared cyclopropyl carbonyl compound has T-type calcium channel regulation activity and has an analgesic effect.

The invention provides a preparation method of viltrabutine hydrochloride, and relates to the technical field of medicine synthesis. The invention relates to a preparation method of viltrobutine hydrochloride, which comprises the following steps: (1) in the presence of a catalyst, reacting 3, 4-dimethoxybenzaldehyde with tert-butyl sulfinamide to obtain a compound VC-1; (2) reacting the compound VC-1 with (3-phenyl propyl) magnesium bromide to obtain a compound VC-2; (3) reacting the compound VC-2 with acid, and neutralizing to obtain a compound VC-3; (4) reacting the compound VC-3 with formaldehyde in the presence of a reducing agent to obtain free viltrabutine; and (5) reacting the free viltrabutine with hydrogen chloride to obtain the viltrabutine hydrochloride. The invention provides a viltrabutine hydrochloride synthesis process which is high in purity, high in yield and simple and convenient to operate, the operation process is simplified, and industrial production is convenient to realize.

The invention discloses a preparation method of 2, 2 '-bis (trifluoromethyl) biphenyl. The invention specifically discloses a preparation method of 2, 2 '-bis (trifluoromethyl) biphenyl, which comprises the following steps of: I, reacting o-chlorobenzotrifluoride with magnesium in a solvent in the presence of lithium chloride, ethyl magnesium bromide and bromoethane to obtain a Grignard reagent; and step II, in a mixed gas atmosphere of oxygen and nitrogen, in the presence of ferric trichloride, carrying out a self-coupling reaction on the Grignard reagent obtained in the step I to obtain 2, 2 '-bis (trifluoromethyl) biphenyl. The raw materials in the synthesis route are cheap and easy to obtain, particularly, the green, cheap and easy-to-obtain mixed gas of oxygen and nitrogen is adopted as the oxidizing agent, and the process yield is high.

A method of producing magnesium cement. The method may comprise mixing water at a temperature of between approximately 50° C. and 100° C., a magnesium oxygen-containing compound and a magnesium salt. In some embodiments, the water is heated to a temperature of between approximately 70° C. and 90° C. The magnesium oxygen-containing compound may comprise one or more of magnesium oxide and magnesium hydroxide. The magnesium salt may comprise one or more of magnesium acetate, magnesium bromide, magnesium oxalate, magnesium thiosulfate, magnesium phosphate, magnesium nitrate, magnesium silicate, a magnesium chloride in any hydration state, anhydrous magnesium chloride, hexahydrate magnesium chloride, a magnesium sulfate in any hydration state, anhydrous magnesium sulfate, heptahydrate magnesium sulfate and magnesium carbonate.

The invention relates to a synthetic method of 2-diphenylmethyl pyrrolidine or an acid salt of 2-diphenylmethyl pyrrolidine. In order to solve the problems of easy ring opening and low yield in the prior art, the invention provides a synthetic method of 2-diphenylmethyl pyrrolidine or an acid salt thereof, which comprises the following steps: in the presence of an alkaline reagent, performing amidation and esterification reaction on a compound pyrrole-2-formic acid as shown in a formula II and ethyl chloroformate in an ROH solvent to obtain a compound as shown in a formula III; r in the ROH solvent is alkyl; performing Grignard reaction with phenyl magnesium bromide to obtain a compound as shown in a formula IV; carrying out reduction reaction on the compound shown in the formula IV under the catalytic action of trifluoroacetic acid and triethyl silane to obtain a compound shown in a formula V; and carrying out hydrolysis reaction on the compound in the formula V under an alkaline condition to obtain the compound 2-diphenylmethylpyrrolidine in the formula I or the acid salt thereof. According to the method, ring-opening impurities can be effectively avoided, the yield is increased to 95% or above, and the purity reaches 99% or above.

The invention discloses anti-mildew plastic for a packaging container and a preparation method of the anti-mildew plastic, and relates to the technical field of plastic. The plastic is prepared from the modified biochar and the modified polyethylene; wherein 3, 5-diformylphenylboronic acid, 5-nitro-2-(oxiranyl methoxy) acetophenone, ethynyl magnesium bromide, isobutyldichlorosilane, hydroxylamine hydrochloride, ammonium salt and 3-butenyl chloroformate are used for synthesizing an anti-aging substance, then the anti-aging substance and polyethylene are subjected to cross-linking modification, an ultraviolet absorption group, a silicon-carbon bond and a boron-carbon bond are introduced into a polyethylene side chain, and the anti-aging substance is prepared. While the photo-thermal aging of the plastic is prevented, the barrier property of the plastic is improved; the biochar is modified by aminopropyl methyl dimethoxysilane, N, N-diethyl-p-aminobenzaldehyde, 11-chlorodecanoic acid and chitosan, antibacterial groups are generated on the surface of the biochar, and the biochar and modified polyethylene can be stacked in order, so that movement of water vapor and oxygen is prevented, and the anti-mildew effect of the plastic is improved.

The application belongs to the technical field of medical intermediates, and relates to a production method of a clotrimazole intermediate (2-chlorophenyl)diphenylmethanol. In the method, 2-methyltetrahydrofuran or cyclopentyl methyl ether is used as a reaction solvent, an ethyl o-chlorobenzoate solution is added dropwise into a phenyl magnesium bromide solution with a concentration of 2.5-3.5 M under the conditions of 60-80 DEG C and inert atmosphere, the reaction is continuously carried out after the dropwise addition is completed, a water solution of a quenching agent is added after the reaction to quench, then, liquid separation is carried out, and the organic phase after the liquid separation is concentrated to obtain a crude product; the crude product is refined by using a reaction solvent and petroleum ether, and (2-chlorophenyl)diphenylmethanol is obtained. The production method can efficiently and stably produce high-quality (2-chlorophenyl)diphenylmethanol, reduces production cost and safety hazards, and can be used for large-scale industrial production.

The invention relates to a preparation method of an alkenyl silane compound, which comprises the following steps: under a protective atmosphere, reacting a silazane compound, an olefin compound, a catalytic amount of titanium catalyst and a catalytic amount of tetrahydrofuran solution of phenyl magnesium bromide or methyl magnesium bromide at 100-120 DEG C for 12-24 hours, and then performing column chromatography purification to obtain the alkenyl silane compound. And the various different substituted alkenyl silane compounds are obtained. The method is simple to operate and low in cost, a series of alkenyl silicon compounds which are difficult to synthesize by a traditional method can be obtained, various compounds can be obtained through further functionalization, and the alkenyl silicon compounds are applied to development and research of medicines and organic functional materials.

The invention provides a preparation process of n-propyl cyclopentadienyl tri (dimethylamino) zirconium. The preparation process comprises the following two steps: step 1, preparing n-propyl cyclopentadiene; the method comprises the following steps: taking a mixture of brominated cyclopentadiene and propyl magnesium bromide as a raw material to react, filtering out solid impurities after the reaction is finished, and carrying out reduced pressure distillation to obtain an n-propyl cyclopentadiene product; step 2, preparation of n-propyl cyclopentadiene tri (dimethylamino) zirconium; according to the method, n-propyl cyclopentadiene and a tetra (dimethylamino) zirconium solution are used as raw materials for reaction, and after the reaction is finished, reduced pressure distillation is performed to obtain n-propyl cyclopentadiene tri (dimethylamino) zirconium. The invention also relates to a film-forming preparation method of the precursor composition, and the precursor composition forms an oxide film, a nitride film or a nitrogen oxide film. According to the invention, the deposition quality defect of the pure propyl cyclopentadienyl tri (dimethylamino) zirconium precursor raw material due to high viscosity is overcome.

A method of producing magnesium cement. The method may comprise mixing water at a temperature of between approximately 50° C. and 100° C. and a magnesium salt to form an intermediate mixture and then mixing the intermediate mixture with a magnesium oxygen-containing compound. The magnesium oxygen-containing compound may comprise one or more of magnesium oxide and magnesium hydroxide. The magnesium salt may comprise one or more of magnesium acetate, magnesium bromide, magnesium oxalate, magnesium thiosulfate, magnesium phosphate, magnesium nitrate, magnesium silicate, a magnesium chloride in any hydration state, anhydrous magnesium chloride, hexahydrate magnesium chloride, a magnesium sulfate in any hydration state, anhydrous magnesium sulfate, heptahydrate magnesium sulfate and magnesium carbonate.

The application belongs to the technical field of cis-jasmone synthesis, and relates to synthesis of a cis-jasmone intermediate, in particular to a preparation method of (Z)-undec-8-ene-2,5-dione. The preparation method comprises the following steps: acetylpropionyl halide and a dihydroxypyrimidine compound are used as starting materials, and (Z)-undec-8-ene-2,5-dione is prepared according to the following reaction route; a solution of (Z)-3-hexenyl magnesium bromide Grignard reagent is uniformly mixed with a solution of a compound shown in formula 3 under the condition of-15-15 DEG C, the temperature is increased to 15-45 DEG C, reaction is carried out for 1-3 hours, the temperature is decreased to 0-5 DEG C and the reaction is quenched, then the pH is adjusted to 1-3 and the temperature is increased to 15-45 DEG C, and reaction is carried out for 2-3 hours; wherein X1 is halogen, X2 is halogen, and R is H or methyl. The preparation method has the characteristics of easy-to-obtain starting materials, higher proportion of isomer Z configuration, simpler operation and the like, and is suitable for industrialized scale production.

The invention belongs to the technical field of synthesis and preparation of organic polymer optical materials, and particularly relates to a cyclotrisulfide-tri (2-mercaptoethyl) thiol composition and a preparation method thereof. The preparation method comprises the following three steps: step 1, performing cyclization and vulcanization reaction on S8 and trichloroethane under the catalysis of aluminum chloride to generate 1, 3, 5-trichlorocyclotrisulfide; step 2, carrying out vinylation reaction on the 1, 3, 5-trichlorocyclotrisulfide and a vinyl magnesium bromide Grignard reagent to generate 1, 3, 5-trivinyl cyclotrisulfide; and 3, carrying out a photocatalytic addition reaction on the 1, 3, 5-trivinyl cyclotripolysulfide and 1, 2-ethanedithiol, and finally synthesizing the cyclotripolysulfide-tri (2-mercaptoethyl) thiol composition. The cyclotripolysulfide-tri (2-mercaptoethyl) mercaptan composition disclosed by the invention is high in transmittance and large in refractive index, and can be used for preparing a polythiocarbamate optical material with a high refractive index and high light transmittance.

The invention relates to the technical field of biological medicines, in particular to a preparation method of an intermediate androstane-17alpha-methyl-17beta-hydroxy-3-ketone of steanoconazole, and belongs to the technical field of biological medicines. The method comprises the following steps: by taking 4-androstenedione as a raw material and p-toluenesulfonic acid as a catalyst, carrying out 3-position ketene etherification protection on the 4-androstenedione and triethyl orthoformate to obtain a compound shown in a formula III; then carrying out Grignard addition on the compound shown in the formula IV and methyl magnesium bromide and carrying out in-situ silyl ether protection to obtain a compound shown in the formula IV; carrying out normal-pressure hydrogenation to obtain a compound as shown in a formula V; and carrying out acid hydrolysis, neutralization, devitrification and recrystallization through a one-pot method to obtain a high-purity target product shown in the formula I. The method is characterized in that the problems of unstable key intermediate, complex process, low yield and the like are successfully solved through in-situ silyl ether protection and one-pot method operation, and the method has the outstanding advantages of short route, safety in operation, high yield, good product purity and suitability for industrial production.

This invention discloses a berberine-dimethylaniline photosensitizer, its preparation method, and its application, belonging to the field of biomedical technology. The method involves sequentially reacting berberine with magnesium methyl bromide via Grignard addition, followed by bromomethylation with N-bromosuccinimide, and basic condensation with dimethylaminobenzaldehyde, then demethylating under high temperature and vacuum to obtain the active berberine-dimethylaniline. Finally, it undergoes weakly alkaline treatment to obtain the inactivated berberine-dimethylaniline. This invention introduces the electron-donating group dimethylaniline onto the berberine backbone, constructing an electron push-pull structure that red-shifts the absorption wavelength, facilitating deeper tissue penetration. Furthermore, this photosensitizer maintains high activity in the weakly acidic microenvironment of tumors while remaining inactive under normal physiological conditions, thereby achieving intelligent "on-off" regulation based on pH differences, improving the safety and precision of photodynamic therapy for tumors.

The invention relates to a preparation method of flurbiprofen with low cost and high purity. The preparation method comprises the following steps: taking 4-bromine-2-fluorobiphenyl as a raw material, and carrying out Grignard reaction on the 4-bromine-2-fluorobiphenyl and magnesium powder to obtain 2-fluoro-4-biphenyl magnesium bromide; the preparation method comprises the following steps: in a solvent, enabling 2-fluoro-4-biphenyl magnesium bromide and N, N-dimethylacetamide to be subjected to a Bouveaut reaction, so as to obtain 2-fluoro-4-biphenyl ethyl ketone; the method comprises the following steps: under the action of a base catalyst, carrying out Wittig reaction on 2-fluoro-4-biphenyl ethanone and (methoxymethyl) triphenyl phosphonium chloride to obtain an alkene etherate, and carrying out acidolysis on the alkene etherate to obtain 2-(2-fluoro-4-biphenyl) propionaldehyde; and carrying out Pinnick oxidation on the 2-(2-fluoro-4-biphenyl) propionaldehyde, sodium chlorite and hydrogen peroxide to obtain racemic 2-(2-fluoro-4-biphenyl) propionic acid, namely, flurbiprofen. The process route totally comprises four steps of reactions, each step is a classical chemical reaction, the HPLC purity of the obtained flurbiprofen is greater than or equal to 99.5%, the materials are cheap and easy to obtain, the operation is simple, the post-treatment is convenient, and the method is suitable for industrial production.

The invention discloses a synthetic method of 7-bromo-5, 6-bis (benzyloxy) benzopyrrole and a derivative dimer of the 7-bromo-5, 6-bis (benzyloxy) benzopyrrole. The synthetic method of the 7-bromo-5, 6-bis (benzyloxy) benzopyrrole comprises the following steps: 1) 2-methoxy-5-nitrophenol is subjected to a bromination reaction through NBS (N-bromosuccinimide), and a compound A is obtained; 2) demethylating the compound A to obtain a compound B; 3) performing benzyl protection on two phenolic hydroxyl groups of the compound B to obtain a compound C; and 4) the compound C is subjected to a Baltorry reaction under the action of vinyl magnesium bromide, and the compound is obtained. The invention relates to a synthesis method of 7, 7 '-dimer, which is characterized in that 7-bromo-5, 6-bis (benzyloxy) benzopyrrole is taken as an initial raw material, and the 7, 7'-dimer is obtained through two-step reaction, the synthesis of the 7, 7 '-dimer is reported for the first time, and the synthesis method has the advantages that the raw material is cheap and easy to obtain, the steps are few, the final product is convenient to purify and easy to stably preserve and the like, and the synthesis method of the 2, 7'-dimer is obviously optimized.

The invention discloses a synthesis method for preparing a fluorine-containing biphenyl compound by a one-pot method, which comprises the following steps: taking fluorine-containing bromobenzene 1A as an initial raw material, reacting with magnesium to generate fluorine-containing phenyl magnesium bromide, reacting with (RO) 3B, hydrolyzing to generate fluorine-containing aryl boric acid ester C, and carrying out coupled reaction with aryl chloride 2A to obtain a target product fluorine-containing biphenyl B; in the formula, R1 is H, F, C1-C6 alkyl and C1-C6 alkoxy; the R group is C1-C6 alkyl, and the R2 group is any one of H, F, C1-C6 alkyl, C1-C6 alkoxy, hydroxyl, nitryl, ester group and carbonyl. According to the method, fluorine-containing bromobenzene is used as a raw material, fluorine-containing phenyl magnesium bromide is prepared from fluorine-containing bromobenzene and magnesium, fluorine-containing phenyl magnesium bromide reacts with boric acid ester and is hydrolyzed to prepare fluorine-containing aryl boric acid ester, and aryl chloride is directly coupled to obtain a target product fluorine-containing biphenyl through a one-pot method without treatment; the method is simple and convenient, can be completed in one pot without post-treatment, and is high in yield and controllable in cost.

The invention discloses a preparation method and application of a series of novel chiral polydentate amino alcohol ligands. The synthesis method comprises the following steps: preparing primary alcohol type chiral amino alcohol by taking L-amino alcohol and 2-halogenated heteroaromatic ring as raw materials and carrying out nucleophilic substitution reaction in one step; the tertiary alcohol type chiral amino alcohol is prepared by taking L-leucine as a raw material, and sequentially carrying out methyl esterification, Buchwald-Harwig cross-coupling reaction and phenyl magnesium bromide addition reaction to synthesize the tertiary alcohol type chiral amino alcohol. The method disclosed by the invention is simple in process, mild in reaction condition, cheap and easily available in raw materials, easy in product separation and purification and high in yield; and the prepared chiral polydentate amino alcohol ligand can be applied to identification of camphorsulfonic acid enantiomers and determination of enantiomer excess (ee value).

The application relates to the technical field of pharmaceutical intermediates, and provides a preparation method of a Resmetirom key intermediate III. The application uses a compound with a structure shown in formula V and a compound with a structure shown in formula E to prepare the Resmetirom key intermediate III, the preparation steps are simple and easy to operate, expensive silver nitrate, cesium carbonate, isopropenyl magnesium bromide and lithium chloride do not need to be used, the product yield is high, the intermediate products are all solid, purification is convenient, moreover, the method provided by the application has small solid waste and waste liquid, is good in environmental protection, finally, the compound with the structure shown in formula G used by the application is stable in property and is not easy to be oxidized. In summary, the method provided by the application can significantly reduce the production difficulty and production cost of the Resmetirom key intermediate III, and is more beneficial to industrialized production.

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a synthesis method of (E, Z)-2, 6-nonadien-1-ol and (E, Z)-2, 6-nonadienal. The method comprises the following steps of: reacting cis-leaf alcohol serving as a starting material with phosphorus oxybromide to generate cis-1-bromo-3-hexene, reacting the cis-1-bromo-3-hexene with magnesium metal to obtain cis-3-hexenyl Grignard magnesium bromide, reacting the cis-3-hexenyl Grignard magnesium bromide with formaldehyde to generate cis-4-heptene-1-alcohol, oxidizing the cis-4-heptene-1-alcohol with sodium hypochlorite under the catalysis of a catalyst 2, 2, 6, 6-tetramethylpiperidine oxide to obtain cis-4-heptene-1-aldehyde, and separating the cis-4-heptene-1-aldehyde from the cis-4-heptene-1-aldehyde. The preparation method comprises the following steps: reacting (E, Z)-2, 6-nonadienoic acid methyl ester with methoxyl formyl methylene triphenyl halophosphine in the presence of potassium tert-butoxide to obtain (E, Z)-2, 6-nonadienoic acid methyl ester, reducing the (E, Z)-2, 6-nonadienoic acid methyl ester with NaBH4 to obtain (E, Z)-2, 6-nonadien-1-ol, and finally oxidizing the (E, Z)-2, 6-nonadienal with sodium hypochlorite under the catalysis of a catalyst 2, 2, 6, 6-tetramethylpiperidine oxide to obtain (E, Z)-2, 6-nonadienal. The method is environment-friendly, low in cost and suitable for industrial production.