47 results about "Silyl ether" patented technology

This invention discloses a chemical preparation method for pharmaceutical-grade dexborneol. The method employs Noyori asymmetric hydrogenation, asymmetric reduction of camphor, and the use of ruthenium as a catalyst. Under the action of phosphine ligands, dexborneol and a small amount of its isomer, isoborneol, are prepared. Then, under the action of trimethylchlorosilane, dexborneol, due to its spatial configuration, can form a silicon-oxygen bond with TMS, while isoborneol cannot. Isoborneol is removed by recrystallization to obtain a silyl ether protected compound of dexborneol. Dexborneol is then prepared under hydrochloric acid conditions and purified by recrystallization to obtain highly purified dexborneol. This route features mild reaction conditions, does not use highly toxic materials, and has a high yield, meeting the requirements for pharmaceutical-grade dexborneol.

This invention belongs to the field of organic synthesis and discloses a method for preparing α-difluoroselenomethyl ketone derivatives using electrochemistry. The method involves preparing α-difluoroselenomethyl ketone derivatives under electrochemical conditions using 2,2-difluorovinyl alcohol trimethylsilyl ether compounds and dialkyl diselenoether. Specifically, the 2,2-difluorovinyl alcohol trimethylsilyl ether compound and the dialkyl diselenoether compound are dissolved in an organic solvent, mixed thoroughly, an electrolyte is added, an inert electrode is inserted, and the reaction is carried out under electrostatic stirring at room temperature to obtain the product α-difluoro(selenomethyl) ketone derivative. This invention eliminates the need for catalysts, bases, persulfates, persulfates, or iodobenzene acetates considered necessary in the prior art; it only requires electrolysis to obtain α-difluoroselenomethyl ketone derivatives in a mild and efficient manner.

The application relates to the field of organic chemistry, in particular to a method for photocatalytic synthesis of silanol or silyl ether. The application provides a method for photocatalytic synthesis of silanol or silyl ether compound, in which, under the condition of existence of an iridium catalyst and an organic solvent, hydrosilane is reacted with any one of water, alcohol or phenol under light to obtain silanol or silyl ether. The synthesis method has high yield and selectivity, low catalyst consumption, mild reaction condition and high environmental protection and efficiency.

The application discloses a kind of thermal stable reworkable polysiloxane elastomer based on silicon ether bond and preparation method thereof, polysiloxane and tetraacid dianhydride are dispersed in solvent respectively, chain extender, tetraacid dianhydride, polysiloxane and modifier are added in sequence and are fully reacted under inert protective atmosphere, then drop in complexing agent, pour into mould after being dispersed uniformly, obtain uncrosslinked product, temperature is raised to 140-200 DEG C and is kept for 5-10h, so that imidization and silicon ether crosslinking occur, then naturally cool to room temperature, obtain target elastomer.The technical scheme of the application reacts amino-terminated polysiloxane with pyromellitic anhydride to obtain polysiloxane long chain, introduces Fe 3+ Coordination bond is used as sacrificial bond to enhance mechanical properties; then dynamic silicon ether bond is used to form dynamic crosslinking network inside material, and polysiloxane elastomer material with good mechanical properties, thermal stability and reworkability is prepared.

The invention relates to a preparation method of a silyl ether composition. The silyl ether composition is prepared from alkyl phenyl silicone oil, polyether, silicon dioxide, an acrylic polymer, a basic catalyst and other raw materials through a certain process. The silyl ether composition can be directly diluted with mineral oil and polyether to obtain a stable mixture which is used as a defoaming agent, and the problem that organic silicon is incompatible with polyether and mineral oil is solved.

The invention discloses a method for preparing cosmetic silicone oil based on an intermediate, which comprises an organic silicon monomer, and the organic silicon monomer is subjected to polymerization reaction under the protection of inert gas by adding a catalyst to produce a silicon-containing intermediate.The method has the beneficial effects that the organic silicon monomer is subjected to polymerization reaction by adding the catalyst; the organic silicon monomer adopts one or any combination of a dimethyl cyclosiloxane mixed ring body, silyl ether, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane, the decamethylcyclopentasiloxane is used as the organic silicon monomer, and the organic silicon monomer is used as the organic silicon monomer, so that the silicon-containing middleware body is formed, and the organic silicon monomer adopts one or any combination of a dimethyl cyclosiloxane mixed ring body, silyl ether, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane. The decamethyl cyclopentasiloxane is a colorless and odorless organosilicon compound, can be used in cosmetics and human body skin care products, and can be well dissolved in most alcohols and other cosmetic solvents, so that the efficiency of preparing cosmetic silicone oil can be improved.

The application discloses a polysiloxane-lignin photo-thermal functional elastomer composite material and a preparation method thereof. After lignin is treated, the lignin is dispersed in a solvent, a modifier and a catalyst are added and reacted to obtain a solid product; the polysiloxane is uniformly dispersed in the solvent, diisocyanate, a chain extender and the modifier are sequentially added and reacted under inert protection atmosphere, a crosslinking agent and the solid product are added to obtain an uncured product, the uncured product is naturally cooled to room temperature after being reacted by heating, a crosslinking product is obtained, the crosslinking product is loaded into a mold and is promoted to crosslink by hot pressing, and the target elastomer is obtained by demolding. The technical scheme of the application reacts amino-terminated polysiloxane with isophorone diisocyanate to obtain a polysiloxane long chain, introduces hydrogen bonds into the material as sacrificial bonds to enhance the mechanical properties; then, a dynamic crosslinking network is formed in the material by using a dynamic silicon ether bond, and the modified lignin added into the material further enhances the mechanical properties of the elastomer and endows the elastomer with excellent photo-thermal conversion function.

The invention relates to the field of biopesticides, in particular to a method for synthesizing sex pheromone of pinus tabulaeformis, which comprises the following steps: reacting 1-bromo-n-heptane (3) serving as an initial raw material with magnesium, and then reacting with (R)-epoxypropane (4) to obtain chiral alcohol 5; then reacting with paratoluensulfonyl chloride, and then reacting with dimethyl malonate to obtain malonate 7; carrying out sodium hydroxide catalytic hydrolysis and high-temperature decarboxylation to obtain an acid 8, and carrying out lithium aluminum hydride reduction and NBS bromination to obtain a chiral bromide 10; reacting with magnesium, and reacting with sulfonate 12 to obtain silyl ether 11; then carrying out TBAF deprotection to obtain chiral alcohol 13; and finally, reacting the chiral alcohol 13 with acetic acid to obtain acetic acid (2S, 3S, 7S)-3, 7-dimethyl-2-pentadecanol ester (1), and reacting the chiral alcohol 13 with propionic acid to obtain propionic acid (2S, 3S, 7S)-3, 7-dimethyl-2-pentadecanol ester (2). The method has the advantages of high total yield, low synthesis cost and the like.

Mixed sulfonyl group-containing co-solvent systems each comprising at least one sulfonyl group-based solvent and one or more non-sulfonyl group-based co-solvents each being a boron-containing solvent, a phosphorus-containing solvent, an ionic liquid solvent, a silyl ether solvent or a derivative thereof, or an isocyanate solvent or a derivative thereof. Specific examples of each type of these non-sulfonyl-based co-solvents are disclosed. Also disclosed are electrolytes comprising the mixed sulfonyl group-containing co-solvent system and one or more alkali metal salts dissolved in the mixed sulfonyl group-containing co-solvent system, as well as alkali metal-based electrochemical cells, battery modules, and batteries containing such electrolytes.

The application discloses a siloxane-linked furan-based dialdehyde compound and a preparation method thereof, and belongs to the technical field of high polymer monomers and material synthesis. 1 and R 2 independently selected from one or more of substituted or unsubstituted C1-C 18 alkyl, 3-7 membered cycloalkyl, C1-C6 alkoxy, C2-C8 alkenyl, substituted or unsubstituted aryl, and X is selected from oxygen or a siloxane structural unit. The siloxane-linked furan-based dialdehyde compound is a potential polymer material monomer, and provides a new idea for biomass-based polymer material synthesis.

The invention relates to the technical field of lithium ion battery electrolyte, and discloses ion polarization enhanced local high-concentration electrolyte and application thereof in a lithium ion battery. The electrolyte contains a lithium salt, a solvent, a diluent and a polarization enhancing component, the polarization enhancing component is neutral molecules, and the molecular polarizability is greater than or equal to 15; the polarization enhancing component is selected from at least one of an aromatic sulfone compound, a conjugated amine oxide, a silyl-containing ether compound and an aromatic amide compound; and in the electrolyte, the concentration of the polarization enhancing component is 0.05 to 2 weight percent. The electrolyte provided by the invention has higher conductivity and lithium ion transference number, the capacity retention ratio of the prepared lithium ion battery is higher, and the high-voltage adaptability is obviously enhanced.

The invention discloses a method for preparing a chiral indazole intermediate (R)-2-amino-3-(7-methyl-1H-indazole-5-yl) methyl propionate of zavazepam, which comprises the following steps of: taking zavazepam as a raw material; the preparation method comprises the following steps: by taking methyl pyruvate as a raw material, generating an enol silyl ether compound of formula IV in situ under the action of a hydrogen pulling reagent and a silicon etherification reagent; coupling the alpha-keto ester compound with a halogenated indazole compound V under the action of a palladium catalyst to obtain an alpha-keto ester compound VI; and finally, carrying out stereoselective transaminase reaction on the compound shown in the formula VI by utilizing specific modified transaminase, so as to efficiently prepare the target chiral intermediate. According to the method, chemical synthesis and biological catalysis are creatively combined, the route only needs three steps, the process is remarkably simplified, the total yield is high, the reaction condition is mild, an expensive chiral catalyst does not need to be used, the yield is remarkably improved by introducing a reaction aid into key steps, and the whole process is easy to amplify and suitable for industrial production.

This invention belongs to the field of pharmaceutical and environmental chemistry, and specifically relates to a method for preparing anacocetate silyl ether. The method for preparing anacocetate silyl ether provided by this invention includes the following steps: (1) 9-hydroxyl elimination reaction, (2) quenching reaction, (3) pH adjustment, (4) dehydration treatment, (5) 17-hydroxyl silyl ether reaction, (6) water washing and layering, (7) concentration and crystallization, (8) solid-liquid separation, and (9) drying. The preparation method provided by this invention achieves a one-pot preparation of anacocetate silyl ether, with a product purity of over 97.5%, isomer content below 0.5%, and molar yield of over 93.4%. This invention features high yield, low pollution, simple and safe operation, and low cost. Furthermore, the preparation method is stable and easily scalable for large-scale industrial 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.

The invention provides a silyl ether-based essential oil compound as well as a preparation method and application thereof. The structural general formula of the compound is Si (R) x (-O-EO) 4-x, and-R is any alkyl or aryl with the carbon number not larger than 6; -O-EO is a plant essential oil active group connected with a silicon atom through an oxygen atom, and the structure of the-O-EO is derived from hydroxyl-containing terpenoids, phenylpropanoid compounds and derivatives thereof in plant essential oil; and x is an integer of 0-3. Through ingenious molecular design, essential oil active molecules are combined with environment-sensitive silyl ether bonds, and effective control over the volatilization and release process of the essential oil is achieved. Experiments prove that the compound has excellent environmental stability and intelligent response release characteristics, can meet the dual requirements of long-acting antibiosis and mildew prevention and lasting fragrance slow release at the same time, and can be widely applied to the fields of intelligent antibiosis, cultural relic protection, food preservation, fragrance slow release systems and the like. Moreover, the preparation method of the silyl ether-based essential oil compound is simple, universal, safe and environment-friendly, and has a wide market prospect.

Described are silyl ether-containing polymers and methods of preparing and using silyl ether-containing polymers, methods of preparing silyl ether-containing polymers, and methods of using silyl ether-containing polymers as a flow control device.

The invention discloses a monofluoro-substituted silyl ether electrolyte material, and belongs to the technical field of lithium battery materials. According to the monofluoro-substituted silyl ether electrolyte material disclosed by the invention, the problems that the voltage of a traditional carbonic ester electrolyte in a lithium metal battery is limited, the cycle rate performance is relatively poor and the like can be solved. The invention discloses a monofluoro-substituted silyl ether electrolyte material, the chemical structural formula of the monofluoro-substituted silyl ether electrolyte material is Rm (R-O) 3-m-(Si-O) n-CH2CH2F, n is an integer of 1 or 2, m is an integer of 1-3, and the-R group is selected from C1-C10 alkyl or fluoroalkyl. The fluorosilyl ether compound has the advantages of high oxidation potential, good lithium metal stability and the like, meanwhile, the binding energy of the fluorosilyl ether compound and Li < + > is small, the solvation ability is weak, and the rate capability of the battery can be effectively improved. The fluorosilyl ether electrolyte material disclosed by the invention can be used as a solvent, an additive or a diluent to be applied to a lithium metal / lithium ion battery, and can also be used as an electrolyte material to be applied to other secondary batteries.

The application relates to the technical field of organic synthesis, and provides a synthesis method of chiral allylamine and application thereof, which takes isoegual and chiral tert-butylsulfonamide as initial raw materials, synthesizes an enamine intermediate M1, adopts a silyl ether protecting group to protect a phenolic hydroxyl group to obtain an intermediate M2, then carries out a Grignard reaction on the intermediate M2 to obtain an intermediate M3, then removes a sulfinyl group from the intermediate M3 to obtain an intermediate M4, and then acetylates to obtain an intermediate M5, and finally removes a silyl ether protecting group from the intermediate M5 to obtain the chiral allylamine. The synthesis method can reduce the preparation cost of the chiral allylamine, is beneficial to industrialized production, optimizes stereoselectivity, and omits a chiral resolution step, and the chiral allylamine can be used for synthesizing colchicine.

The application discloses anthraquinone-based polysulfate and a preparation method and photocatalytic application thereof, and belongs to the field of polymer material synthesis and photocatalytic technology. The polysulfate takes 2,6-dihydroxyanthraquinone derivative as a core monomer, is connected through a sulfate bond to form a conjugated polymer, and has excellent visible light absorption capacity and electron transport performance. The preparation method takes 2,6-dihydroxyanthraquinone as a starting material, synthesizes a double silyl ether protected anthraquinone intermediate and a thiofluoride activated anthraquinone intermediate respectively, and finally performs polycondensation on the two intermediates under a potassium hydrogen fluoride / crown ether catalytic system. The material can catalyze hydrogen peroxide to be generated from water and oxygen under visible light irradiation, and the yield reaches 2667 μmol·h ‑1 ·g ‑1 , is a new type of efficient photocatalytic material, and has wide application prospects in the fields of green synthesis and environmental catalysis.

The invention discloses a preparation method of basic nickel carbonate in the field of inorganic material preparation. The method comprises the following steps: mixing a nickel sulfate solution and a sodium carbonate solution in a reaction kettle, adding a specific molecular regulating agent, carrying out precipitation reaction at a controlled temperature, aging, filtering, washing and drying to obtain sphere-like basic nickel carbonate with uniform granularity and high purity. The regulating agent is synthesized by the following steps: firstly, protecting hydroxyl of (S)-tert-leucinol by using tert-butyldimethylsilyl chloride; then carrying out Michael addition with 2-(trifluoromethyl) acrylic acid under the action of a basic catalyst; carrying out secondary Michael addition on the obtained product and 2-dodecenoic acid to introduce a hydrophobic long chain; removing a silyl ether protecting group to release hydroxyl; and finally salifying with sodium hydroxide to obtain the target regulating agent. The molecular regulating agent can effectively control the precipitation process through steric hindrance and coordination, significantly improves the particle size distribution and purity of the product, and is simple in preparation process and suitable for industrial production.

The present disclosure provides permanently charged cationic lipids that are particularly beneficial in formulations of lipid nanoparticles providing advantageous improvements in the delivery of nucleic acids to hepatic stellate cells with enhanced efficiency. The permanently charged cationic lipids are quaternary ammonium lipids that are silyl ethers. The disclosure also provides lipid nanoparticle, pharmaceutical compositions, and methods including the provided permanently charged cationic lipids.

A surface recovery process that restores the hydrophobicity of dielectric surfaces and promotes selective deposition of metal-fill such as molybdenum onto metal-containing surfaces while reducing or preventing growth on the dielectric surfaces. Additionally, the surface recovery process reduces film loss against subsequent wet etching processes such as DHF. The recovery precursor soak is performed with optional UV (concurrent or sequential) to react with silanols on damaged dielectric surface to replenish -CHS and recover hydrophobicity of the dielectric surface. The recovery precursor is a carbon-containing recovery precursor, for example, organohalosilanes, esters, silyl ethers, organoaminosilanes, silyl esters, hydrocarbons, or a combination thereof.

The application belongs to the technical field of lithium ion batteries, and discloses a ternary high-voltage lithium ion battery nonaqueous electrolyte and a lithium ion battery. The ternary high-voltage lithium ion battery nonaqueous electrolyte comprises a nonaqueous organic solvent, an electrolyte lithium salt and a film-forming additive, the film-forming additive comprises a cyano compound containing a silicon ether structure, and the cyano compound containing the silicon ether structure has a structural formula as shown in formula (I): wherein the substituents R1 and R2 are each independently selected from alkyl, alkenyl, fluoroalkyl, phenyl and cyanoxyl with 1-4 carbons. The lithium ion battery nonaqueous electrolyte has high energy density and high safety performance through optimization of a formula and under the joint action of various components in a unique combination, and is beneficial to meeting the demand of the electrolyte on cycle performance under high voltage.

The invention discloses a high-performance two-component flame-retardant waterproof polystyrene foam and a preparation method, and relates to the technical field of building waterproof materials, the high-performance two-component flame-retardant waterproof polystyrene foam comprises a component A and a component B, and the mixing ratio of the component A to the component B is 1: 1 by mass; the component A is prepared from the following components according to the total mass: a silicon-ether-epoxy hybrid prepolymer, polyether polyol 3030K, nano microencapsulated ammonium polyphosphate and organic phosphorus modified polyol. According to the invention, a silyl ether epoxy hybrid curing technology and a nanoscale composite flame-retardant synergistic strategy are adopted, so that the defects in the prior art are effectively overcome. A system framework is constructed through a silyl ether epoxy hybrid prepolymer, and the flexibility of polyether polyol is combined, so that the product has high bonding strength and good elasticity, the elongation can reach 50% or above, and the tensile bonding strength with concrete is greatly enhanced. A nanoscale composite flame-retardant system has a synergistic effect, so that the flame-retardant property of the product reaches UL-94 flame-retardant grade of V-0, and the influence of a large amount of filled flame retardant on foaming and mechanical properties is avoided.

The application discloses a preparation method of natural products Pancratinine B and C and intermediates thereof. The preparation method of a key intermediate compound 8 comprises the following steps: 1) compound 1 is reacted with a nitrogen iodine compound to obtain compound 2; 2) compound 2 is subjected to a cycloaddition reaction with a compound 2' protected by a silicon-based protecting group R1 to obtain compound 3; 3) compound 3 is formed into an enol silyl ether, and then subjected to Saegusa-Ito oxidation to obtain compound 4; 4) compound 4 is subjected to a reduction reaction to obtain compound 5; 5) compound 5 is subjected to hydroxyl protection to obtain compound 6; 6) compound 6 is subjected to deprotection of a group R to obtain compound 7; and 7) compound 7 is subjected to a Pictet-spengler condensation reaction to obtain compound 8. Then, Pancratinine C and B are prepared from compound 8 via compounds 9 and 10 respectively. The method is a brand-new synthesis method, the reaction route is simple, the reaction condition is mild, and the method is easy to operate.

This invention discloses an industrial-scale chemical preparation method for 1,2-di fatty acid glycerides, comprising the following steps: (A) acetone glycerol is protected with a silyl ether protecting agent and purified by crystallization to obtain intermediate 1; (B) intermediate 1 undergoes a depropionyl protecting group reaction and crystallization to obtain intermediate 2; (C) intermediate 2 undergoes an esterification reaction and crystallization and adsorption to obtain intermediate 3; (D) intermediate 3 undergoes a desilyl ether protection reaction and recrystallization to obtain 1,2-di fatty acid glycerides. This invention, through crystallization purification under different conditions, avoids the disadvantages of traditional chemical methods for preparing 1,2-di fatty acid glycerides, such as the need for multiple column chromatography purification steps, low yield, and difficulty in industrialization. This method features mild operating conditions, high purity, and is easily scalable for large-scale industrialization.

This application discloses a composite bipolar plate, its preparation method, and a fuel cell. The preparation method includes: reacting graphite material under nitrogen and hexamethyldisilazane vapor conditions to obtain modified graphite; wet mixing resin and modified graphite to obtain a composite material; and pressing and curing the composite material to obtain the composite bipolar plate. This application modifies the graphite material using HMDS, causing the hydroxyl groups on the graphite surface to react with HMDS to form silane-ether bonds, and also grafting CH3 from HMDS onto the graphite surface. The silane-ether bonds and the grafted CH3 enhance the chemical bonding between graphite and resin, thereby enhancing the compatibility and bonding force between graphite and resin, improving the mechanical strength and airtightness of the composite bipolar plate, and facilitating the preparation of thinner composite bipolar plates.

The invention relates to a 2N-type cobalt complex and a preparation method thereof. The 2N-type cobalt complex is used for a silylation reaction of hydrogen-containing silane and alcohol. The invention relates to a 2N type cobalt complex, and the 2N type cobalt complex is one of Co < 1 >-Co < 6 >. According to the 2N type cobalt complex, the preparation method thereof and the silylation reaction of the hydrogen-containing silane and the alcohol, the 2N type cobalt complex can be used for catalyzing the silylation reaction of the hydrogen-containing silane and the alcohol to synthesize the triphenyl silyl ether, and has the advantages of mild conditions, simple synthesis steps, lower cost, higher catalytic activity, good substrate universality, no need of an active auxiliary agent and the like; and a new method is provided for constructing the silicon-oxygen bond.

The invention discloses a mixed mode chromatographic stationary phase based on cyclic polyamine and a preparation method thereof, N-monoalkylated piperazine is firstly obtained through a selective N-alkylation technology, then the N-monoalkylated piperazine is converted into silane, then the silane is immobilized on silica gel, and the novel mixed mode chromatographic stationary phase based on cyclic polyamine is prepared. Selective N-alkylation adopted in the method has reaction specificity, silane synthesis has diversity, and the obtained stationary phase has remarkable alkalinity, excellent hydrophilicity and stability, is suitable for analyzing high-activity electrophilic reagents, weakens the tendency that a silyl ether bond between a bonded phase and a silica gel substrate is damaged by a protonic solvent in a mobile phase, and improves the stability of the stationary phase. Loss of a chromatographic stationary phase is reduced, and the chromatographic retention capacity is improved.

The invention discloses a method for synthesizing furan derivatives under the catalysis of copper, which comprises the following steps: in an organic solvent system, by taking silyl enol ether compounds as shown in a formula (1) as raw materials, metal copper salt as a catalyst, metal silver salt as a cocatalyst, metal potassium salt as alkali and tert-butyl peroxide as a free radical initiator, stirring and reacting at 120 DEG C, and tracking and detecting through TLC (Thin Layer Chromatography) until the reaction is complete, thereby obtaining the furan derivatives. And performing post-treatment on the reaction liquid to obtain the furan derivative as shown in the formula (2). The method is simple to operate, reagents are easy to obtain, reaction conditions are mild, a reaction system is green and environment-friendly, products are easy to separate and purify, the method is suitable for synthesizing various highly-functionalized furan derivatives, and the high-purity furan derivatives can be efficiently prepared.