233 results about "Magnesium bromide" patented technology

The invention discloses a preparation method of LCZ696 intermediate and relates to the technical field of preparation of an aromatic nucleus compound containing 2 benzene rings and 1 chiral center. The preparation method includes the steps of S1, allowing benzyl magnesium bromide to react with methyl oxalyl chloride to obtain a compound as shown in formula I; S2, allowing the compound as shown in formula I to have a bromination reaction with a bromination reagent to generate a compound as shown in formula II; S3, coupling the compound as shown in formula II with phenylboronic acid to obtain a compound as shown in formula III; S4, performing reductive ammoniation on the compound as shown in formula III to obtain a compound as shown in formula IV; S5, applying Boc to the compound as shown in formula IV to obtain a compound as shown in formula V; S6, performing ester group reduction on the compound as shown in formula V to obtain a compound as shown in formula VI. The preparation method has the advantages that overall raw material consumption is lowered, and product productivity and market competiveness are increased; by the overall process optimization, the reaction of each step can be performed and controlled easily, the use of heavy metal catalysts is reduced and avoided, and accordingly the quality index of the final product is increased, and an economic and environment-friendly process route is developed.

The invention provides a method for preparing propargyl alcohol by using a micro-structural reactor, which comprises the steps of by taking a simple Grignard reagent as a raw material, carrying out gas-liquid Grignard exchange reaction on the simple Grignard reagent and acetylene gas to generate a high-quality acetylene-based magnesium bromide Grignard reagent, carrying out nucleophilic addition reaction on the obtained acetylene-based magnesium bromide Grignard reagent and an electrophilic reagent in a continuous flow condition, and carrying out hydrolysis, separation and refining on the product to obtain a substitution propargyl alcohol product. The method provided by the invention has the advantages that the operation is simple, the raw material and the reagent are simple, cheap and easily available, the process is continuous, rapid and controllable, the condition is mild, the product has good selectivity and industrial production can be realized.

The invention relates to a comprehensive treatment method of seawater or strong brine. The comprehensive treatment method comprises the following steps: pretreatment, low-interception nanofiltration separation, low-interception nanofiltration permeate liquid treatment, reverse osmosis concentrated water treatment, nanofiltration osmosis permeate liquid treatment and nanofiltration concentrated water treatment. According to the method, fresh water is completely recycled, the yield of low-value magnesium chloride and calcium sulfate (gypsum) byproducts is greatly reduced, low-value sodium sulfate, magnesium bromide and the like are prevented from being generated, and the yield of high-value products such as high-purity sodium chloride, calcium chloride, potassium sulfate and magnesium sulfate is remarkably increased.

The invention relates to a method for preparing an Invokana key intermediate. By utilizing a complex of transitional metal nickel, the catalytic cross coupling reaction on 2-bromothiophene and p-fluorophenyl magnesium bromide is realized, and the problem that the existing palladium catalyzing method for synthesizing the Invokana key raw material 2-(4-fluorophenyl) thiophene is high in cost is solved.

In an embodiment of the present disclosure, a method for fabricating a sugar product is provided. The method includes mixing formic acid and lithium chloride, magnesium chloride, calcium chloride, zinc chloride or iron chloride or lithium bromide, magnesium bromide, calcium bromide, zinc bromide or iron bromide or heteropoly acid to form a mixing solution, adding a cellulosic biomass to the mixing solution for a dissolution reaction, and adding water to the mixing solution for a hydrolysis reaction to obtain a sugar product. The present disclosure also provides a sugar product fabricated from the method.

Provided is a metal halide lamp capable of being dimmed, which is prevented from non-lighting due to leakage of an arc tube attributable to a crack occurring at thin tubes, as well as realizing a desired color characteristic. The metal halide lamp has an arc tube that includes an envelope made of translucent ceramic, a pair of electrodes, and metal halides, the metal halides including rare earth metal halide, sodium halide, and magnesium halide, the rare earth metal halide being at least one of dysprosium halide, thulium halide, holmium halide, cerium halide, and praseodymium halide, and the magnesium halide being at least one of magnesium iodide and magnesium bromide, where when a maximum lamp power P (W) is in a range of 70 W to 250 W, the following relations are satisfied: 0.0345A+0.0028B<0.0015P+0.0475; A≧0.021P+0.313; and B≧10.0, where A (mg) represents a total content of the metal halides, and B (mol %) represents a content ratio of the magnesium halide to the metal halides.

An efficient anticorrosion coating for metal pipes is prepared from raw materials in parts by weight as follows: 12-18 parts of fluorosilicon resin, 4-7 parts of clam shell powder, 8-20 parts of inorganic filler, 2-3 parts of a curing agent, 6-13 parts of a nano oxide particle reinforcing agent, 7-10 parts of flaky aggregate, 5-9 parts of rust resisting pigments, 2-4 parts of a thickener, 8-14 parts of silica powder, 4-7 parts of anti-cracking pigments, 6-10 parts of an organic solvent, 2-4 parts of a coalescing agent, 5-8 parts of phenolic aldehyde modified amine, 13-16 parts of a solvent and 1.5-2.4 parts of magnesium bromide. The efficient anticorrosion coating has the benefits as follows: the efficient anticorrosion coating for the metal pipes has good high-temperature resistance and oxidation resistance and high chemical stability and has a good market prospect, and the preparation process is simplified.

The present invention is one kind of 2-substituted rubrene compound as shown and its synthesis process. The synthesis process includes the first synthesis of 2-formoxyl rubrene, and the subsequent oxidation, reduction and condensation with 2-formoxyl rubrene to obtain other 2-substituted rubrene compound. The synthesis process of 2-formoxyl rubrene under protection of inert gas includes the first reaction of 2-formoxyl -6, 11-diphenyl-5, 12-tetracene quinine material with glycol and catalyst at 120-160 deg.c; the subsequent reflux reaction with phenyl magnesium bromide and anhydrous tetrafuran; and final reflux reaction with iron powder and glacial acetic acid under heliophobic condition to obtain 2-formoxyl rubrene. The 2-substituted rubrene compound of the present invention as new type of red fluorescent material has high fluorescence quantum efficiency and may be used as the luminous material in electroluminescent device.

The invention discloses a β-diimine monovalent magnesium compound and its preparation and application in silanization of aldehydes and ketones. The preparation method is as follows: under anhydrous and oxygen-free conditions, β-diimine ligand reacts with Grignard reagent to generate magnesium bromide, and then reduces it with sodium to obtain yellow crystal, which is β-diimine monovalent magnesium compound. The β-diimine monovalent magnesium compound of the present invention has simple synthesis, convenient separation and purification, clear structure, and high yield; it has high activity as a catalyst to catalyze the reaction of aldehydes or ketones with trimethylsilyl cyanide, and the substrate is universal wide sex.

The invention relates to synthesis of 4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-hydroxymethyl benzonitrile. The synthesis comprises the following steps: 1) dispersing 5-cyano isobenzofuranone into a solvent for optimizing a Grignard reaction, adding a p-fluorophenyl magnesium bromide solution, and performing a primary Grignard reaction, wherein the solvent is chlorinated hydrocarbon, ethanediol diether, 1,3-propanediol diether, 1,4-butanediol diether or 1,4-dioxane; 2) continuing to add a 1-(3-(N, N-dimethylamino) propyl) magnesium chloride solution, and performing a secondary Grignard reaction to obtain a mixed reaction solution; and 3) performing posttreatment on the mixed reaction solution to obtain 4-[4-(dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl]-3-hydroxymethyl benzonitrile. By the synthesis method, generation of byproducts is effectively inhibited and the yield and the purity of the target product are improved.

The invention discloses a preparation method of ulipristal acetate and an intermediate thereof, and belongs to the field of pharmaceutical synthesis. The preparation method of the ulipristal acetate comprises the following steps: by taking 3,3-(ethylenedioxy)-19-methylestra-5(10),9(11)-diene-3,17-diketone as raw material, enabling the raw material to react with sodium acetylide or potassium acetylide to obtain a compound III, carrying out high-selectivity epoxidation by oxide to obtain a compound IV, subsequently enabling the compound IV to react with 4-(N,N-dimethyl amino) phenyl magnesium bromide Grignard reagent to obtain a compound V, then enabling the compound V to react with phenyl sulfonic acid chloride to obtain a compound VI, enabling the compound VI to respectively react with sodium methoxide and trimethyl phosphate to obtain a compound VII, hydrolyzing and removing a protection group to obtain a compound VIII, finally carrying out acetylation reaction to obtain the ulipristal acetate, wherein the reaction formulae are as shown in the description. The method is short in synthetic route, mild in reaction conditions, high in yield and purity of products, low in cost, stable and controllable in quality, and is suitable for industrial production.

The invention discloses a preparation method of an organism in chemical industry technical field, in particular to the preparation method of a 2, 6-Dimethyl-2-Heptanol. The invention is that: firstly methylic Grignard reagent is prepared through taking Benzyl magnesium Chloride or Benzyl magnesium Bromide as an initiator, then is carried out the Grignard reaction with 2-Methyl-2-Hepten-6-Ketone, and finally is catalyzed and hydrogenated to synthesize 2,6-Dimethyl-2-Heptanol. The initiator prepared by the invention has the advantages of relatively stable property, easy preservation, higher initiating speed compared with commonly used initiator, strong universality, low dosage, convenient storage and low toxicity, etc. The initiator is especially suitable for preparing Grignard Reagent in mass production. The product prepared by the invention has better security and higher yield. The prepared product can be widely used in essence prescription of daily chemistry.

The invention discloses a chlorine dioxide disinfectant special for livestock and poultry, which belongs to the technical field of disinfection. The product is prepared from the following raw materials in parts by weight: chlorite, monopersulfate, an acidifying agent, bromide salt, a stable forming agent and a drying agent. The chlorite is at least one of alkali metal salt of chlorite and alkalineearth metal salt of chlorite; the acidifying agent is at least one of sodium hydrogen sulfate, sodium bicarbonate, potassium bicarbonate and boric acid; wherein the bromide salt is selected from at least one of sodium bromide, lithium bromide, potassium bromide, calcium bromide, magnesium bromide, ammonium bromide and aluminum bromide; wherein the stable forming agent comprises at least one of sodium sulfate, magnesium sulfate, magnesium hydroxide, sodium chloride and magnesium chloride; and the drying agent is at least one of calcium chloride, calcium sulfate and calcium stearate. The invention also provides a preparation method of the disinfectant. The disinfectant does not generate substances such as chloroform and cyanuric acid in the activation process, so that the disinfectant is suitable for occasions such as livestock and poultry breeding.

The invention discloses a method for preparing cyclopropylboric acid. The method comprises the following steps: reacting cyclopropyl bromide with magnesium reagents to generate cyclopropylmagnesium bromide which then reacts with 1-substituent boronic acid pinacol ester to prepare cyclopropylboric acid. The raw materials for the method are easy to obtain, the operation is easy, the method is safe and environment-friendly, the cost is low, and the yield is high. The innovation includes that hazardous materials such as lithium metal and diethyl ether in the literature are avoided; and cyclopropylmagnesium bromide and 1-substituent boronic acid pinacol ester are taken as the raw material to synthesize cyclopropylboric acid with a high yield under the room temperature condition, therefore the raw material risk is small, the reaction conditions are mild, the yield is high, and the environment is not polluted.

The invention discloses a preparing method of 3-alkoxy phenylcarbinol, comprising the steps: (1) dissolving 3-bromobenzene alkyl ether into a solvent, thus generating a Grignard reagent (3-alkoxy) phenyl magnesium bromide with Mg under the action of an initiator; (2) adding paraformaldehyde into the Grignard reagent at 50-85 DEG C to generate a substitution product; (3) performing acid hydrolyzing on the substitution product to obtain 3-alkoxy phenylcarbinol. Raw materials adopted in the invention are lower in price, the preparing method is mild in reaction conditions, only post-treatment of one time is required after three steps of reaction, and operation time is short; the purity of the obtained 3-alkoxy phenylcarbinol is high and completely accords with the requirements on use as a medicine intermediate.

The invention discloses a preparation method of 1-bromoalkyne and 1-iodoalkyne. The preparation method comprises the following steps that terminal alkyne is adopted as a raw material, a chloramine salt and an iodine salt or a bromine salt is adopted as a halogenation system, and reaction is carried out in a solvent to synthesize a series of 1-bromoalkyne and 1-iodoalkyne type compounds. In the formula shown in the description, R in terminal alkyne is selected from chain-like alkyne, ring-shaped alkyne, olefin, ester group, cyanogroup, substituted phenyl group and heterocyclic arene; the chloramine salt is selected from one of chloramine B, chloramine T or o-chloramine T; the iodine salt is selected from one of sodium iodide, potassium iodide, ammonium iodide, lithium iodide or tetrabutylammonium iodide; the bromine salt is selected from one of sodium bromide, potassium bromide, lithium bromide, magnesium bromide, ammonium bromide or tetrabutylammonium bromide; the solvent is selected from one or is mixed by two of water, benzene, methylbenzene, 1, 4-dioxane, ethyl acetate, dimethyl sulfoxide, methanol, tetrahydrofuran, alcohol, isopropyl alcohol, N, N-dimethyl formamide, n-pentane,dichloromethane, petroleum ether, methyl tert-butyl ether, chloroform, n-hexane, carbon tetrachloride, n-butyl alcohol, 1,2-dichloroethane or acetonitrile. The preparation method disclosed by the invention has the beneficial effect that the application is wide.

The invention relates to a method for preparing a 3-(alkoxy phenyl) bismuth serial compound. An alkoxy brombenzene serial compound is used as a raw material; under the protection of nitrogen gas, the alkoxy brombenzene serial compound in an anhydrous solvent and magnesium chips are subjected to Grignard reaction to generate an alkoxy phenyl magnesium bromide Grignard reagent; and the alkoxy phenyl magnesium bromide Grignard reagent and anhydrous bismuth trichloride undergo metal transferring reaction to prepare the 3-(alkoxy phenyl) bismuth serial compound. The alkoxy brombenzene serial compound comprises p-BrC6H4OMe, o-BrC6H4OMe, p-BrC6H4OEt, o-BrC6H4OEt or m-BrC6H4OEt. An organic solvent with high boiling point is safer than aether and can activate the magnesium chips; in particular, THF is adopted to emulsify and dissolve anhydrous BiCl3 and is favorable for preparation operation; the reclaimed THF can be used for subsequent extraction, save raw materials and reduce pollution; and the method has mild reaction condition and uncomplicated technical requirement, and is favorable for industrialized preparation.

The invention discloses a preparation method of mestanolone. The structural formula of the mestanolone is as shown in the specification. The specific preparation method comprises the following steps of (1) generating a compound II with cyan from a compound I and acetone cyanohydrin or sodium cyanide; (2) adjusting a solution of the compound II into acidity, tracking ethylene glycol and triethyl orthoformate into ketal, adjusting the solution into strong basicity to form a compound III; (3) adding a catalyst and hydrogen to the solution of the compound III to generate a compound IV; (4) putting the compound IV into a container and dissolving by using tetrahydrofuran, dropping a Grignard reagent of methylmagnesium chloride or methyl magnesium bromide to obtain a compound V; and (5) elutriating the compound V in the same container under an acid condition to obtain 3-ketal, namely mestanolone. Chemical production of the mestanolone is achieved by adopting the simplest process, the required raw materials are few, the pollutants are few, meanwhile, the produced mestanolone is high in purity and the relative yield is increased.

The invention discloses a method for catalytic synthesis of salidroside. The method comprises the following steps: enabling total acetyl glucose to react with 4-benzyloxy-phenethyl alcohol under the action of a catalyst to obtain 2-(4-benzyloxyphenyl)ethyl-(2,3,4,6-O-tetra-acetyl)-beta-D-glucopyranoside, wherein the catalyst is tin chloride, zinc oxide, aluminum trichloride, boron fluoride or copper chloride, or a mixture of one of tin chloride, zinc oxide, aluminum trichloride, boron fluoride and copper chloride as well as magnesium fluoride, magnesium chloride, magnesium bromide or magnesium iodide; and removing an acetyl protective group from the product in the presence of an organic base to obtain 2-(4-benzyloxyphenyl)ethyl-beta-D-glucopyranoside, and introducing hydrogen into 2-(4-benzyloxyphenyl)ethyl-beta-D-glucopyranoside under the catalysis of palladium and carbon to perform reduction reaction so as to remove a benzyl protective group, thereby obtaining 2-(4-hydroxyphenyl)ethyl-beta-D-glucopyranoside. The method disclosed by the invention has the outstanding characteristics that the yield is high, the total acetyl glucose is subjected to three steps of reaction, the total yield can reach 63%, the process is simple, the cost is low, and the method is suitable for industrial mass production.

The invention relates to a method for preparing a safe and effective antibechic dimimorfan phosphate. The method comprises steps of reacting dextrorphane with trifluoro-methylsulfonyl chloride in triethylamine so as to generate dextrorphane trifluoro-methyl sulfone chloride ester; reacting the dextrorphane trifluoro-methyl sulfone chloride ester with tetramethyltin in methylbenzene so as to generate (9s, 13s, 14s)-3, 17-dimethyl morphinan (or adding the dextrorphane trifluoro-methyl sulfone chloride ester into mixed solvent of THF and N-methyl-2-pyrrolidone, adding catalyst ferric acetylacetonate and methyl magnesium bromide, stirring and heating reflux for 12 hours, so as to prepare (9s, 13s, 14s)-3, 17-dimethyl morphinan), furthermore, reacting with phosphoric acid so as to salify to prepare target product (9s, 13s, 14s)-3, 17-dimethyl morphine phosphate-dimimorfan phosphate. The method takes commercially available dextrorphane as the raw material, and prepares the target product through three steps of esterification, methylation and salification. The method has advantages of easily obtained raw materials, few synthesis steps, simple technology, low cost, high yield, high purity of the product and strong economic practicability, and is applicable to industrial production.

The invention discloses a novel byproduct produced by an ethinyloestradiol synthesis process and a synthesis method thereof. The byproduct is as shown in a formula I, and the chemical name is 3-hydroxy-19-nor-17alpha-pregna-1,3,5(10)-triene-20-(3-hydroxy-3-methylbutynyl-1-yl)-17-ol. The invention also provides a preparation method of the byproduct. The substance can be simply and conveniently obtained by performing Grignard exchange on alkyl magnesium bromide and 3-methyl-1-butynyl-3-ol and then performing Grignard exchange on estrone. The compound can be used as a standard substance for controlling impurities in an ethinyloestradiol production process.

The invention relates to an anti-aging corrosion-resistant plastic and wood composite material plate, which is prepared from the following ingredients in percentage by weight: 5 percent to 10 percent of plant fiber, 10 percent to 15 percent of magnesium bromide, 20 percent to 25 percent of polystyrene, 3 percent to 5 percent of aluminum hydroxide, 5 percent to 10 percent of basic magnesium sulfate whiskers, 20 percent to 25 percent of wood flour, 1 percent to 2 percent of alkyl sodium sulfonate and 5 percent to 8 percent of phthalic anhydride. The invention also provides a preparation method of the anti-aging corrosion-resistant plastic and wood composite material plate. The method comprises the following steps of mixing the ingredients; performing melt blending by an extruding machine and performing granulation; performing cold pressing and shaping for preparing the anti-aging corrosion-resistant plastic and wood composite material plate. The manufacturing is convenient; the cost is low; the plastic consumption and the wood consumption are low; the environment-friendly effect is achieved; the anti-corrosion performance is realized; the service life is long. The anti-aging corrosion-resistant plastic and wood composite material plate can be widely applied to various fields. The anti-aging corrosion-resistant plastic and wood composite material plate prepared by the method has the anti-aging and anti-corrosion performance; the preparation method is simple; the raw materials can be easily obtained.