32 results about "Magnesium iodide" patented technology

The invention discloses an asymmetric beta-diimine univalent magnesium complex as well as a preparation method and an application thereof in a hydroboration reaction of nitrile. The preparation methodcomprises the steps as follows: firstly, acetylacetone and 2,6-diisopropyl aniline are condensed and then react with 2,4,6-trimethylaniline to produce an asymmetric beta-diimine ligand, then the asymmetric beta-diimine ligand reacts with the same amount of methylmagnesium iodide to produce magnesium iodide, finally, the magnesium iodide is reduced with excessive sodium, and the asymmetric beta-diimine univalent magnesium complex is obtained. The preparation method is simple, the synthesized asymmetric beta-diimine univalent magnesium complex has the high yield and has significant effects in the hydroboration reaction of nitrile, the reaction condition is mild, the reaction speed is high, the yield can reach 90% or above, and a catalyst has very high activity.

The invention relates to a method for synthesizing a secondary metabolite of blue algae-2-methylisoborneol (the full name is 1,2,7,7-tetramethyl-outer-double ring-[2,2,1]-2-enanthol). The method comprises that d-camphor and organic compounds of magnesium (methyl magnesium iodide) are subjected to alkylation reaction to synthesize the 2-methylisoborneol, wherein the methyl magnesium iodide is prepared by the reaction of iodomethane and metal magnesium in absolute ethyl ether. The invention also relates to a method for removing impurities from the synthesized product and purifying and identifying the 2-methylisoborneol.

The invention discloses an unsymmetrical β-diimine monovalent magnesium compound, a preparation method thereof and an application in aldehyde and ketone hydroboration reactions. Its preparation method is as follows: first condense acetylacetone with different kinds of aromatic amines respectively to generate asymmetric β-diimine ligands, then react it with an equal amount of methylmagnesium iodide to generate magnesium iodide, and finally use excess The sodium reduction of unsymmetrical β-diimine monovalent magnesium compound. The preparation method of the invention is simple, and the synthesized asymmetric β-diimine monovalent magnesium compound has a remarkable effect in the hydroboration reaction of aldehydes and ketones, and the catalyst consumption is only 0.1%, the reaction speed is fast, the yield is very high, and it is highly in line with green Chemistry concept.

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 discloses a method for preparing alkaline type magnesium iodide crystal whiskers. The method comprises the following steps: S1, taking bittern, filtering and discarding insoluble substances; S2, mixing a NaI solution with concentration of 3 mol/L with a bittern solution treated in step S1 in a volume ratio of 3 to 1 to obtain a mixed solution 1; S3, heating the mixed solution 1 to 30 DEG C, then dropwise adding a NaOH solution with concentration of 0.8 mol/L into the mixed solution 1 under a stirring state to obtain a mixed solution 2, wherein a volume ratio of the mixed solution 1 to the NaOH solution with concentration of 0.8 mol/L is (2.5-3.5) to 1; and S4, continuously ageing the mixed solution 2 for 55 hours at a temperature of 35 DEG C, filtering and collecting precipitates, and drying the precipitates to obtain the alkaline type magnesium iodide crystal whiskers.

The invention discloses a fluorine-containing organosilicone monomer and a preparation method thereof. The method is characterized in that the method comprises the steps that 3-tridecafluorohexyl propylene and tridecafluoro-1-iodohexane are taken as starting materials, and undergo a single electron transfer addition reaction to synthesize 1,3-bi-(tridecafluorohexyl)-2-iodopropane; 1,3-bi-(tridecafluorohexyl)-2-iodopropane reacts with magnesium metal to prepare 1,3-bi-(tridecafluorohexyl)-2-propyl magnesium iodide which further reacts with silicon tetrachloride to form fluorine-containing alkyl-substituted chlorosilane; and a bi-[1,3-bi-(tridecafluorohexyl) isopropyl] dichloro-silicohydride product is obtained by recification. In a molecular structure of the product, perfluoroalkyl is short-chain perfluoroalkyl; the length of a carbon chain is equal to 6; the product is not degraded difficultly, has no cumulative toxicity, and is an environment-friendly monomer for synthesizing fluorine-containing polysiloxane. The preparation and reaction conditions of the fluorine-containing organosilicone monomer are mild; a technique is simple and convenient; the raw materials are easy to obtain; and industrialized production, and popularization and application are facilitated.

The invention discloses a phase change energy storage material capable of recycling, which comprises calcium dichloride, potassium fluoride, manganese nitrate, magnesium iodide, sodium sulfate, sodium acetate, lithium chlorate, sodium carbonate, Water, the proportion of each component of the recyclable phase change energy storage material is: in parts by weight, 5-10 parts of calcium dichloride, 8-12 parts of potassium fluoride, 13-17 parts of manganese nitrate, Magnesium iodide 11-15 parts, sodium sulfate 7-12 parts, sodium acetate 3-7 parts, lithium chlorate 10-15 parts, sodium carbonate 4-8 parts, water 30-35 parts. Through the above method, the present invention can achieve a very good phase change energy storage effect through the compound use of several inorganic substances, the material can be recycled, and it still has a very good effect after multiple cycles, saving the cost of use. Energy is saved.

The invention discloses a synthesis method of tetraethylene silane, and relates to the technical field of battery electrolyte additives, and the synthesis method comprises the following steps: under the protection of an inert gas, dissolving tetrachlorosilane in methyl tert-butyl ether, adding a catalyst magnesium iodide, slowly dropwise adding a vinyl magnesium chloride solution into the obtained system, carrying out a Grignard reaction, and after the reaction is completed, carrying out a reaction to obtain the tetraethylene silane. And adding water for quenching, performing phase splitting, and performing vacuum concentration on the obtained organic phase to obtain the tetraethylene silane. The synthesis method provided by the invention is simple to operate, few in reaction steps and easy to purify, the product yield and the product purity in the production process are ensured to be maximized by controlling reaction conditions in each stage, and the product yield is further improved by reasonably controlling the dosage of reaction raw materials and the reaction process.

The invention discloses a chemical phase analysis method for passivated magnesium. The chemical phase analysis method comprises the following steps: utilizing the characteristic that the magnesium metal in a specimen can take a reaction with iodine to generate magnesium iodide to be dissolved in methyl alcohol, so as to effectively separate out the magnesium metal from the specimen, enabling the magnesium oxide in the precipitate to take a reaction with nitric acid, putting the reactant in a solution, respectively carrying out EDTA (Ethylene Diamine Tetraacetic Acid) developing titration on the solution dissolved with the magnesium metal or magnesium oxide, so as to obtain the content of the magnesium metal and the magnesium oxide. The chemical phase analysis method disclosed by the invention is quick, accurate, efficient, and simple in operation, and has better practicability.

The invention discloses a preparation method of a caine drug intermediate (S)-2-piperidinecarboxylic acid. The preparation method specifically comprises the following steps of a) carrying out a one-pot reaction on 5-chlorovaleraldehyde, L-phenylglycinol and trimethylsilyl cyanide under the action of a catalyst A to obtain a compound as shown in a formula (I), wherein the catalyst A is magnesium diiodide, magnesium dibromide and magnesium perchlorate, (b) carrying out catalytic hydrogenation reaction on the compound as shown in the formula (I) to obtain (S)-2-cyano piperidine as shown in a formula (II), and (c) hydrolyzing the compound as shown in the formula (II) to obtain (S)-2-piperidinecarboxylic acid as shown in a formula (III). The preparation method utilizes cheap and easily available organic raw materials, and has the advantages of simple operation, mild reaction conditions, good stereoselectivity, high yield and the like.

The invention discloses a total-deuteration tert butyl alcohol preparation method which comprises the following steps: firstly, making deuterium methyl magnesium iodide and deuteration acetone performGrignard reaction in anhydrous tetrahydrofuran under the existence of anhydrous manganese chloride; then hydrolyzing a reaction product under the acid condition to generate total-deuteration tert butyl alcohol, wherein the acid condition is formed by a heavy water solution which deuteration acid is added in. The total-deuteration tert butyl alcohol preparation method disclosed by the invention has the advantages of moderate reaction condition, high reaction yield, ability in obtaining abundant total-deuteration tert butyl alcohol and simpleness in technological operation.

The invention discloses a method for synthesizing 6-bromomethyl-3-methoxy-2-nitropyridine. The method comprises the synthesizing steps: firstly, mixing 6-methyl-3-hydroxyl-2-nitropyridine, magnesium iodide and water, dropwise adding dimethyl sulfate, carrying out a reaction for 24 hours with heating, carrying out extraction with ethyl acetate, and boiling off the ethyl acetate, so as to obtain 6-methyl-3-methoxyl-2-nitropyridine; and adding carbon tetrachloride and sodium bromide, carrying out stirring for dissolving, dropwise adding hydrogen peroxide, carrying out a reaction with heating, boiling off the carbon tetrachloride, adding 200ml of water, carrying out extraction with ethyl acetate, boiling off the ethyl acetate so as to obtain crude 6-bromomethyl-3-methoxyl-2-nitropyridine, carrying out column chromatography separation, and carrying out recrystallization with acetonitrile water, thereby obtaining the 6-bromomethyl-3-methoxy-2-nitropyridine. According to the method, the yieldis 75%.