155 results about "Trimethyl borate" patented technology

The invention belongs to the field of medicine synthesis and specifically relates to a preparation method of an anidulafungin side chain intermediate 4'-orthopentyloxy-1,1':4',1'-terphenyl-4-carboxylic acid. The preparation method comprises the following steps: initiating a 1,4-dibromo-benzene material which serves as a starting material to carry out Grignard reagent reaction with magnesium by iodine; then, preparing 1,4-benzene hypoboric acid by virtue of addition and hydrolysis with trimethyl borate; and preparing 4'-orthopentyloxy-1,1':4',1'- terphenyl-ethyl carboxylate by virtue of Suzuki reaction of 1,4-benzene hypoboric acid, 4-pentyloxy bromobenzene and 4-halogenated ethyl benzoate in dioxane-ethanol liquor under catalysis of [1,1'-bis(diphenyl phosphino) ferrocene] palladium dichloride, and then, hydrolyzing to obtain a target product. The preparation method disclosed by the invention can lower process cost, is simple, convenient, safe and reliable to operate, and suitable for industrial production.

A novel carbinol gasoline fuel relates to an engine fuel, in particular to a novel liquid fuel for a gasoline engine. According to the weight parts, the novel carbinol gasoline fuel is mixed simply by the following raw materials of the composition: 20-80 of gasoline, 20-90 of carbinol, 2-10 of petroleum ether, 1-5 of 2-methylpentane, 0-5 of octane, 0-5 of isooctane, 0-5 of diethyl carbonate, 0-4 of cinnamene, 0.2-4 of trimethyl borate, 0-5 of dibutyl phosphite, 0.5-5 of dimethyl carbonate, 0-5 of methyl tertiary butyl ether, 0-4 of ether, 0-4 of isopropyl ether, 0-6 of acetone, 0-4 of isopropyl alcohol, 0-5 of isobutyl alcohol and 0-4 of anti-oxidant. The antiknock index is reinforced as the octane number is improved; and the compounding is optimized scientifically during the experiment and practice, thus leading the vehicle to keep the best stability on all aspects when the liquid fuel is in use.

The invention relates to a method for fast preparing boron carbide ceramic powder. The method for fast preparing the boron carbide ceramic powder comprises the following steps: 1) choosing raw materials: choosing trimethyl borate and sucrose according to the weight ratio of the trimethyl borate to the sucrose equal to (12:1)-(12:3); choosing methanol, chelating agent acetic acid and water according to the volume ratio of the trimethyl borate, the methanol, the chelating agent acetic acid to the water equal to (6:40:1:1)-(6:80:2:4); and choosing solvent acetic acid according to the ratio of the sucrose to the solvent acetic acid equal to (7-8)g:50ml; 2) preparing dry gel powder; 3) preparing precursor powder; and 4) thermally treating the precursor powder. Under the conditions of high heating speed and short heat preserving time, the carbon thermal reduction reaction is carried out so that the carbon thermal synthesis process of the boron carbide is shortened to dozens of minutes or even several minutes; and, high-purity fine carbon carbide ceramic powder with good sintering property can be obtained without the subsequent carbon removal processes. The carbon carbide ceramic powder is the single carbon carbide phase through X-ray diffraction analysis; the content of free carbon in the product is 1-3%; and, the grains are uniform and fine, and the average grain size is less than 500nm.

The invention relates to a triphyene derivative containing diarylethene and an application thereof. The triphyene derivative is obtained by the way that triphyene derivative halogeneated triphyene and bisthienylethenes containing trimethyl borate are in coupled reaction. The designed and compounded triphyene derivative has the characteristics of being good in heat stability, high in quantum efficiency, short in light response time and the like. In addition, a unique solvation color development phenomenon is shown in triphyene derivative alkane chloride. Consequently, the triphyene derivative containing the diarylethene not only can be used for full color display and information storage but also can be used for trace detection of the alkane chloride.

The invention discloses a method and a special device for separating trimethyl borate from a carbinol mixture. The method is a salt-adding extraction and rectification method which comprises the following steps of: charging a salt-containing solvent, trimethyl borate and carbinol mixture from the upper part and middle part of an extraction and rectification tower respectively, carrying out salt-adding extraction and rectification, withdrawing pure trimethyl borate from the top of the tower, and obtaining the mixture of carbinol, salt and solvent at a tower kettle; and charging the mixture of carbinol, salt and solvent into a solvent recovering tower from the middle, wherein the distillate on the top of a recovery tower is the carbinol, obtaining the salt-containing solvent at the tower kettle, and repeatedly charging the salt-containing solvent into the extraction and rectification tower to be used. The method is better in effect due to the salt-adding extractant compared with the extractant, has the advantages of being convenient to recycle and easy to realize on the industry, can be used for overcoming the defect that the sold salt in a salt-adding rectification technology is hard to cycle, can be used for greatly improving the separation effect since the relative volatility of the trimethyl borate and the carbinol is increased, has the advantages of being low in equipment investment and low in energy consumption, and can be used for the industrial application for the separation and purification of the trimethyl borate.

The invention provides a preparation method of tri(pentafluorophenyl) borane. The method comprises the following steps: by using pentafluorobromobenzene as a raw material, dissolving the raw material in an organic solvent; adding strong base at a certain temperature; reacting to obtain an intermediate; and performing a reaction on the intermediate and trimethyl borate for a period of time to obtain tri(pentafluorophenyl) borane. The preparation method provided by the invention has the characteristics of shorter reaction process, simpleness and convenience in operation and lower cost of raw materials.

The invention discloses a preparation method of trimethyl borate. The method comprises the following steps of: (1) heating and dehydrating a boric acid solid to prepare metaboric acid and pyroboric acid solids; (2) adding the metaboric acid and pyroboric acid solids which are obtained in the step (1) to methanol to make the mixture react under a stirring state; (3) heating and distilling the reaction solution obtained in the step (2) to obtain an azeotrope solution of the methanol and the trimethyl borate, distilling and cooling raffinate to obtain boric acid; and (4) separating the azeotrope solution of the methanol and the trimethyl borate, which is obtained in the step (3), to obtain a trimethyl borate product. In the invention, by firstly heating and dewatering the boric acid to prepare the metaboric acid and the pyroboric acid and then making the metaboric acid and the pyroboric acid react with the methanol to prepare trimethyl borate, the reaction speed is accelerated, the conversion per pass is improved, the reaction conditions are mild and no risks exist.

The invention provides a synthetic method for tetra(pentafluorophenyl)borate. The synthetic method comprises the following steps: with pentafluorobromobenzene as a starting raw material, treating pentafluorobromobenzene with organic lithium or a Grignard reagent so as to obtain an intermediate A; reacting the intermediate A with trimethyl borate; and carrying out post-treatment so as to obtain the target product tetra(pentafluorophenyl)borate with a structural formula described in the specification. M+ in the product of the method is any one selected from the group consisting of organic carbocation, organic ammonium ion and alkali metal ion. Compared with the prior art, the invention has the following advantages: usage of tri(pentafluorophenyl)borane sensitive to water and oxygen is avoided; product yield is high; and the method has good process and operation practicality, simple steps and low requirements on equipment and is suitable for industrial production.

The invention discloses a preparation method of 4-phenoxyphenylboronic acid, which relates to the technical field of organic synthesis. It uses 4-bromodiphenyl ether as a raw material and tetrahydrofuran as a solvent to react with magnesium flakes to prepare Grignard reagent, and the obtained Grignard reagent is react with trimethyl borate, hydrochloric acid hydrolysis to obtain crude 4-phenoxyphenylboronic acid, and finally obtain the finished product of 4-phenoxyphenylboronic acid after purification. The raw materials used in the invention are cheap and easy to obtain, the reaction conditions are mild, the post-treatment operation is simple, the production cost is low, the yield is high, and the method is suitable for industrial production.

A composition comprising a polyepoxide, a hardener, trimethyl borate, and a flame retardant is disclosed. Methods for preparing the composition and its end uses are also disclosed.

The invention discloses a nano silicon dioxide modified wood production method including five steps of pretreatment, preparation of a wood modification agent, preparation of a wood modification fluid, dipping treatment and post-drying treatment, wherein the wood modification agent comprises nano silicon dioxide, fatty alcohol polyoxyethylene ether, distilled water, trimethyl borate, dodecyl dimethyl benzyl ammonium chloride, N-(2-benzimidazole)-methyl carbamate, and imidacloprid. The beneficial effect is that the nano silicon dioxide modified wood production method has the advantages of simple treatment process, easy operation, low cost, good treatment effect, no toxicity, environmental friendliness and the like, the treated wood has no obvious appearance change, and wood dimensional stability, density, surface hardness, bending strength and bending elastic modulus, good processing properties, wear resistance, anti-corrosion flame retardant properties are greatly increased.

The invention discloses a preparation method for 3-carboxyphenylboronic acid, relating to the technical field of organic synthesis. The preparation method comprises the steps of performing Grignard reaction on m-bromomethyl benzene, magnesium scraps and iodine by using the m-bromomethyl benzene as a starting material, so as to generate a Grignard reagent, performing boronated reaction on the Grignard reagent and trimethyl borate so as to prepare 3-Tolylboronic acid, and oxidizing the 3-Tolylboronic acid with potassium permanganate in an alkaline condition so as to prepare 3-carboxyphenylboronic acid. According to the preparation method, cheap m-bromomethyl benzene easy to obtain is used as the starting material, the 3-carboxyphenylboronic acid is prepared through Grignard reaction, boronated reaction and oxidization reaction, the operations are simple, the average purity of the product 3-carboxyphenylboronic acid reaches 99.3%, and the average total yield reaches 50%. The product yield and purity are ensured at low cost, so that the preparation method is applicable to industrial production.

The invention discloses a preparation method of crisaborole. The method comprises the steps as follows: a compound shown in a formula I and alkali metal borohydride are subjected to a contact reaction, and a compound shown in a formula II is obtained; the compound shown in the formula II and a compound a are subjected to a contact reaction, and a compound III is obtained; or the compound shown inthe formula II and dihydropyran are subjected to a contact reaction, and a compound III is obtained, wherein the compound a is trimethylchlorosilane, tert-butyldimethylsilyl chloride or chloromethyl methyl ether; the compound shown in the formula III and an isopropylmagnesium chloride solution are subjected to a contact reaction, and a standby solution is obtained; then, the standby solution is added to a mixed solution of a compound b and a third organic solvent for a contact reaction, hydrochloric acid is added for a contact reaction, and crisaborole, namely, a compound shown in a formula IV, is obtained, wherein the compound b is 2-alkoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane, triisopropyl borate or trimethyl borate.

The invention relates to a preparation method of boron-10 acid. The preparation method of the boron-10 acid comprises the following steps: heating a prepared lithium carbonate-water solid-liquid mixture to be at 40-80 DEG C, inflating boron trifluoride-10 gas into the lithium carbonate-water solid-liquid mixture, stirring so as to uniformly disperse the boron trifluoride-10 into the solid-liquid mixture, and stopping gas inflation when the mol ratio of the boron trifluoride-10 to the lithium carbonate reaches (1: 1.5)-1.6; conducting an reaction for 10-25 hours to generate the boron-10 acid; separating, and performing ion exchange and crystallization to separate out the boron-10 acid solid. The preparation method is carried out in an aqueous system, thus avoiding ester hydrolysis in the process of generating trimethyl borate; the preparation method is simple in process and can be industrialized easily; the boric acid is high in yield and purity, the yield is above 95% and the purity is above 98%.

Fuel mixtures for direct methanol fuel cells are disclosed. The fuels include methanol and additives that react with water to produce methanol and other easily electro-oxidizable compounds including dimethyloxymethane, methylorthoformate, tetramethylorthocarbonate, trimethylborate, and tetramethylorthosilicate. Other additives to improve safety and efficiency of the fuel cell include sulfonated activated carbon particles and metal hydrides, such as LiAlH₄, NaBH₄, LiBH₄, (CH₃)₂ NHBH₃, NaAlH₄, B₂H₆, NaCNBH₃, CaH₂, LiH, NaH, KH or sodium bis (2-methoxyethoxy) dihydridaluminate.

A wood treating agent is prepared from the following raw materials in part by weight: 3-10 parts of phenol, 4-7 parts of melamine, 5-10 parts of potassium isopropoxide, 5-8 parts of calcium chloride, 3-8 parts of phosphoric acid, 3-5 parts of boric acid, 1-4 parts of zinc chloride, 6-10 parts of trimethyl borate, 7-10 parts of dodecyl dimethyl benzyl ammonium chloride, 5-9 parts of lignin, 4-8 parts of waterborne zinc stearate emulsion, 5-11 parts of sodium tripolyphosphate, 2-6 parts of folic acid, 3-9 parts of parachlorometaxylenol, 8-11 parts of bronopol, and 6-8 parts of sodium chlorate. The wood treating agent has the benefits that the wood treating agent has good corrosion prevention and insect prevention effects, can form a good breathable layer, and can prolong the service life of wood.

The invention provides a preparation method of diborane, and solves the technical problems of unreasonable preparation method, high raw material price, complex product purification operation, high cost, low yield and unsuitability for industrial production. The preparation method of diborane takes sodium hydride, trimethyl borate and boron trichloride as initial raw materials, and tetrahydrofuran as a reaction solvent, and carries out condensation reaction and a double decomposition reaction to obtain the diborane. The method can be widely applied to the technical field of diborane preparation.

A process for preparing phenylboric acid includes two steps: preparing Grig nard reaction liquid and preparing phenylboric acid. In the second step, the tributyl borate is used to replace trimethyl borate, resulting in high output rate (more than 60%) and low cost.

The invention provides a pickling-free flux, comprising 37-47% of trimethyl borate (by weight); preferably, the weight percentage of the trimethyl borate is 40%. The invention also provides a method used for preparing the pickling-free flux, comprising the steps as follows: under the conditions of temperature of 45-50DEG C, the pressure of 1Pa-1.2Pa and the catalyst of potassium permanganate, boracic acid and carbinol react completely, filtrated and washed to a neutral state, thus gaining the pickling-free flux; furthermore, the pickling-free flux is dried suitably. The pickling-free flux has simple and convenient usage, good film-forming effect, no residues after brazing and no corrosion phenomenon occurring on brazing workpiece, reduces the brazing cost, and protects the environment; the preparation method is simple and convenient and the gained product has high purity.

A method is provided for recovering boric acid from a solution containing boric acid and at least one lithium compound. The method comprises (a) passing the solution through an ion exchange resin such that boric acid accumulates on the resin; (b) removing the boric acid from the resin with an aqueous alcohol solution, thus obtaining a first solution comprising an alcohol, boric acid, and water; (c) converting at least a portion of the boric acid to trimethyl borate, thereby obtaining a second solution; (d) distilling an azeotrope from the second solution, wherein the azeotrope contains trimethyl borate; and (e) recovering boric acid from the azeotrope.

The 7-amino-3-methoxymethyl-3-cephem-4-carboxylic acid of molecular formula (I) can pass through the azeotropy of 7-aminocephalosporanic acid of molecular formula (II) and trimethyl borate and methyl alcohol The mixture is readily prepared by reaction in the presence of methanesulfonic acid.

The invention discloses a preparation method of a Crisaborole intermediate. The Crisaborole intermediate has a structure shown as the formula VI. The preparation method comprises the following steps:performing a contact reaction on a compound shown as the formula I and benzyl halide, so as to form a compound shown as the formula II; performing a contact reaction on the compound shown as the formula II and alkali metal borohydride, so as to obtain a compound shown as the formula III; performing a contact reaction on the compound shown as the formula III and a compound a, or performing a contact reaction on the compound shown as the formula III and dihydropyran, so as to obtain a compound shown as the formula IV, wherein the compound a is trimethylchlorosilane, tert-butyldimethylsilyl chloride and chloromethyl methyl ether; performing a contact reaction on the compound shown as the formula IV and an isopropylmagnesium chloride solution; adding an obtained solution into a compound b, performing a contact reaction on the mixture and fourth organic solvent mixed liquor and adding hydrochloric acid into the mixture for contact reaction, so as to obtain a compound shown as the formula V,wherein the compound b is 2-alkoxy-4, 4, 5, 5-tetramethyl-1, 3, 2-dioxaborolane, triisopropyl borate or trimethyl borate; performing a hydrogenation reaction on the compound shown as the formula V toobtain a compound shown as the formula VI.