39 results about "Magnesium bromide" patented technology

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 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 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.

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 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 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.

This invention relates to a method for preparing 1,4,5,8-tetramethoxynaphthalene compounds containing the characteristic side chain of shikonin and their 6-fluoro derivatives. The method uses 2-fluoro-1,4-dimethoxybenzene or 2,5-difluoro-1,4-dimethoxybenzene as starting materials. After cyclization, ring-opening, and O-methylation to construct the 1,4,5,8-tetramethoxynaphthalene core, an aldehyde group is introduced at the 2-position via Vilsmeier-Haack formylation. This is followed by addition with allyl magnesium bromide to obtain an allyl alcohol intermediate. Finally, a cross-metathesis reaction catalyzed by a Grubbs II catalyst is performed with 2-methyl-2-butene to construct the characteristic side chain of shikonin –CH(OH)CH2CH=C(CH3)2. This invention offers high yields, simple operation, avoids the use of highly toxic reagents, and successfully solves the problem of the difficulty in synthesizing 6-fluoro derivatives due to direct fluorination, providing a key intermediate for the development of novel naphthoquinone drugs.

The invention relates to a metal organic gel type composite adsorbent as well as a preparation method and application thereof. The metal organic gel type composite adsorbent comprises metal organic gel and hygroscopic salt, the hygroscopic salt comprises any one or a combination of at least two of calcium chloride, magnesium chloride, sodium chloride, barium chloride, cesium chloride, lithium bromide, calcium bromide, magnesium bromide, sodium bromide, barium bromide or cesium bromide. According to the preparation method of the metal organic gel type composite adsorbent, synthesis conditions are mild, large-scale preparation is easy, a reaction product is blocky gel, a final product is a granular integral adsorbent after drying, the adsorbent has efficient water vapor adsorption capacity, and the adsorbent has good application prospects. The metal organic gel type composite adsorbent has excellent adsorption and desorption performance and good cycle stability on water vapor.

The invention relates to the technical field of metal plates, in particular to an aluminum alloy plate and application thereof in nuclear power engineering. The aluminum alloy plate consists of 70wt%-75wt% of aluminum alloy powder and 25wt%-30wt% of ionic liquid functionalized boron carbide, wherein the functionalized boron carbide is prepared by loading 1-hydroxyethyl-3-methylimidazolium magnesium bromide on the surface of boron carbide; through ionic liquid functionalization treatment, interface bonding of boron carbide and an aluminum matrix is improved, and the mechanical property of the material is improved; the high-temperature stability of the material is enhanced through the synergistic effect of hydroxyethyl functional groups and magnesium ions; meanwhile, the surface electron state of boron carbide is optimized, and the neutron absorption cross section of the material is reduced. The invention solves the problems of insufficient mechanical property, poor high-temperature stability, high neutron absorption rate and the like of the traditional aluminum alloy in nuclear power application, and is particularly suitable for the fields such as nuclear reactor components with harsh requirements on material performance.

The invention discloses a preparation method and a detection method of hinokitiol, and belongs to the technical field of synthesis of medical intermediates, the preparation method comprises the following steps: S1, carrying out a reaction on cyclopentadiene, ethyl magnesium bromide and isopropyl p-toluenesulfonate to obtain cyclopentadiene; the preparation method comprises the following steps: carrying out an addition reaction on 1-isopropyl cyclopentadiene and dichloroacetyl chloride in a solvent to prepare 7, 7-dichloro-3-isopropyl-bicyclo [3, 2, 0] hept-2-ene-6-one, and carrying out a reaction on the 7, 7-dichloro-3-isopropyl-bicyclo [3, 2, 0] hept-2-ene-6-one and 1-isopropyl cyclopentadiene in the solvent to prepare 7, 7-dichloro-3-isopropyl-bicyclo [3, 2, 0] hept-2-ene-6-one; s3, the 7, 7-dichloro-3-isopropyl-bicyclo [3, 2, 0] hept-2-ene-6-ketone, a mixed solution containing tert-butyl alcohol, acetic acid and water and triethylamine are subjected to a ring expansion reaction, and a crude product of hinokitiol is prepared; and S4, carrying out alkali extraction and acid precipitation on the hinokitiol crude product, and recrystallizing to obtain hinokitiol. The method greatly simplifies the post-treatment process, has the advantages of low cost, high purity, high yield and the like, and is suitable for large-scale industrial production.

This invention relates to a method for preparing mandelic acid derivatives. The invention uses commercially available conventional p-chlorophenyl magnesium bromide reagent as raw material, which is low in cost, readily available, and reduces raw material costs by more than 40%. Furthermore, the synthesis steps are simple, low in cost, low in toxicity, convenient to operate, and highly safe.

The invention relates to the field of the oil production industry, and more particularly to heavy well kill fluids containing at least one of the compounds: calcium bromide, barium bromide, magnesium bromide, strontium bromide, zinc bromide, calcium iodide, barium iodide, magnesium iodide, strontium iodide and zinc iodide, and to methods for producing same. The invention discloses a method which makes it possible to broaden the range of components that can be used to produce heavy kill fluids. The claimed method makes it possible to produce a heavy well kill fluid using accessible salt solutions, wherein the resulting fluid has the necessary properties for effectively killing wells. The claimed method includes mixing solutions of salts at a molar ratio of 0.5-1.3:2, evaporating the resulting mixed solution to a density of 1400-2650 kg / m3, cooling the evaporated solution to a temperature of less than 25°C to form a precipitate, and filtering the evaporated solution to obtain a filtrate in the form of a heavy well kill fluid.

The invention discloses 2-isopropyl-5-(4, 4, 5, 5-tetramethyl-1, 3, 2-dioxaborolane-2-yl) thiazole and a synthesis method and application thereof.The synthesis method of the 2-isopropyl-5-(4, 4, 5, 5-tetramethyl-1, 3, 2-dioxaborolane-2-yl) thiazole comprises the steps that S1001, a compound 1, namely 2, 5-dibromo thiazole and zinc salt are added into a first organic solvent, the mixture is stirred at the room temperature, a reaction is conducted for 2-4 hours, and a second organic solvent is obtained; the preparation method comprises the following steps: slowly adding an isopropyl magnesium bromide solution under the protection of inert gas, adding a catalyst after the addition is completed, heating to 40-60 DEG C, slowly adding the isopropyl magnesium bromide solution, stirring and reacting at 40-60 DEG C for 0.5-2 hours, cooling the system to-60--40 DEG C, adding isopropyl alcohol pinacol borate, slowly adding the isopropyl magnesium bromide solution, stirring and reacting at 40-60 DEG C for 0.5-2 hours, cooling the system to-60--40 DEG C, cooling to-60--40 DEG C, adding the isopropyl alcohol pinacol borate, stirring and reacting at 40-60 DEG C for 0.5-2 hours, stirring and reacting for 1-3 hours at the temperature of-60 DEG C to-40 DEG C; and S1002, after the reaction is completed, carrying out post-treatment on a reaction solution, so as to obtain the 2-isopropyl-5-(4, 4, 5, 5-tetramethyl-1, 3, 2-dioxaborolane-2-yl) thiazole, namely the 2-isopropyl-5-(4, 4, 5, 5-tetramethyl-1, 3, 2-dioxaborolane-2-yl) thiazole.

The application belongs to the technical field of organic synthesis, and particularly relates to 5-acetyl-1H-pyrazole-3-carboxylic acid and a preparation method and application thereof. The preparation method comprises the following steps: firstly, reacting raw material 3,5-pyrazole dicarboxylic acid and tert-butyl alcohol to obtain intermediate a; then, reacting the intermediate a with N,O-dimethylhydroxylamine hydrochloride to obtain intermediate b; then, reacting the intermediate b with methyl magnesium bromide to obtain intermediate c; finally, hydrolyzing the intermediate c by using alkali liquor, and neutralizing the product by using acid to obtain 5-acetyl-1H-pyrazole-3-carboxylic acid. The raw material used in the reaction is easy to obtain, the reaction condition is mild, the operation is simple, the total yield of the product is greater than 70%, the purity of the product reaches more than 99.9%, and the method is suitable for large-scale industrial production.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of 2-(4-(cyclopropyl formyl) phenyl)-2-methyl tert-butyl propionate 13C. Comprising the following steps: introducing carbon dioxide (13C) into tetrahydrofuran and a reagent A at-80 DEG C to synthesize cyclopropanecarboxylic acid (13C), wherein the reagent A is cyclopropyl magnesium bromide and cyclopropyl magnesium iodide: adding the cyclopropanecarboxylic acid (13C), dichloromethane, dimethyl hydroxylamine hydrochloride and 4-dimethylaminopyridine into triethylamine at room temperature, and reacting at the temperature of-80 DEG C to obtain the cyclopropanecarboxylic acid (13C). The preparation method comprises the following steps: synthesizing N-methoxy-N-methyl cyclopropanecarboxamide-13C from 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride; the preparation method comprises the following steps: adding 2-(4-bromophenyl)-2-tert-butyl methyl propionate and tetrahydrofuran into a reaction kettle, dropwise adding an alkali solution at the temperature of-40 DEG C, and dropwise adding N-methoxy-N-methylcyclopropanecarboxamide-13C to synthesize 2-(4-(cyclopropanecarboxyl) phenyl)-2-tert-butyl methyl propionate-13C, thereby obtaining the 2-(4-(cyclopropanecarboxyl) phenyl)-2-tert-butyl methyl propionate-13C. The method is reasonable in route, low in cost, high in yield and easy to industrialize.

The invention relates to the technical field of medical chemical medicines, in particular to a novel synthesis method of cis-chiral alpha-hydroxy-beta-amino acid hydrochloride. The preparation method comprises the following steps: taking cheap and easily available natural alpha-amino acid as a starting raw material, firstly, preparing N-Boc protected amino aldehyde 2 from the natural alpha-amino acid as the starting raw material, then carrying out Grignard reaction on the N-Boc protected amino aldehyde 2 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 N-Boc protected amino aldehyde 2. And performing stereospecific ring closing to obtain trans-oxazolidine 3. The compound 3 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 4. And finally, carrying out reflux deprotection by using 6N hydrochloric acid to obtain the cis-chiral alpha-hydroxyl-beta-amino acid hydrochloride. The synthetic route is convenient to operate, the total yield is high, and large-scale preparation can be achieved.

The application discloses a boron-nitrogen doped polycyclic aromatic compound and a synthesis method thereof, and relates to the technical field of organic synthesis. The application takes o-bromonitrobenzene as raw material, and first carries out a Bartoli reaction with vinyl magnesium bromide to synthesize 7-bromoindole; then carries out twice coupling reactions under the action of a metal catalyst to form a dimer of indole; carries out a reaction of the dimer of indole with di-tert-butyl dicarbonate to obtain a single Boc dimer of indole; carries out a borohydration reaction on the single Boc dimer of indole to obtain a boron-containing intermediate; and finally carries out a reaction with a Grignard reagent to obtain the boron-nitrogen doped polycyclic aromatic compound. The synthesis method has the characteristics of a relatively short reaction path, simple operation method and mild reaction conditions. Meanwhile, the compound synthesized by the application is sensitive to fluoride ions and has a high fluorescence quantum yield, and can be applied to the fields of fluoride ion sensors and organic photoelectric materials, and has a wide application prospect.

This invention discloses a curcumin derivative with therapeutic effects on acute lung injury and its preparation method, comprising: dissolving curcumin in tetrahydrofuran, removing air from the reaction apparatus, and adding nitrogen to the reaction apparatus to fill it with nitrogen; then adding ethyl magnesium bromide and refluxing at a first preset temperature for 30 min; then adding succinic anhydride and refluxing at a second preset temperature for 4 h; stopping the reaction by adding water and adjusting the pH to 4 with hydrochloric acid; after extraction with ethyl acetate, purifying the upper layer using a preset method to obtain a yellow oily substance I-1; reacting curcumin succinate monoester I-1 with a 5% sodium bicarbonate solution, and evaporating the solvent to obtain curcumin succinate monoester sodium salt II. The raw material used in this invention has wide clinical applications and is safe and low in toxicity. The hydroxyl group of curcumin is combined with succinic anhydride through a Grignard reaction to form curcumin succinate monoester I-1, which is then reacted with sodium bicarbonate solution to obtain curcumin succinate monoester sodium salt II.