93 results about "Silyl ether" patented technology

The invention discloses a novel method for synthesizing 1, 3-diketone organic matters, which comprises the following steps: by taking acyl chloride and silyl enol ether as raw materials, generating acyl free radicals through photo-induced copper catalysis, and carrying out free radical addition reaction on the acyl free radicals and silyl enol ether, thereby efficiently constructing 1, 3-diketone compounds. Compared with strong base, oxidant, high temperature and expensive metal catalyst required by the existing method, the method provided by the invention adopts the cheap and high-yield copper catalyst, so that the production cost is reduced, and the economic benefit is improved. In addition, the method has mild reaction conditions, easily available catalysts and raw materials, utilizes clean and sustainable light energy as driving force, is simple and convenient to operate, and is suitable for large-scale production. The invention provides an economic and environment-friendly innovative way for synthesizing the 1, 3-diketone compound, and has a wide application prospect.

The present invention provides a poly(O,O'-monothiocarbonate) compound and its preparation method and application, belonging to the technical field of sulfur-containing polymers. The present invention carries out a polymerization reaction of silyl ether, elemental sulfur and difluorocarbene reagent under the action of an organic base, dissolves the obtained polymer product in an organic solvent and adds a precipitant for precipitation, and the obtained precipitate is a poly(O,O'-monothiocarbonate) compound. The poly(O,O'-monothiocarbonate) compound prepared by the present invention has a clear chain structure, and the prepared film refractive index reaches 1.6188, with outstanding optical properties; and the reaction raw materials of the preparation method of the present invention are easily available and can be directly purchased commercially, with the advantages of low raw material price, mild synthesis conditions, simple process and high polymerization efficiency.

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.

The invention discloses and requests to protect a preparation method of high-purity norbornene alkyl silyl ether. Specifically, the invention discloses and requests to protect an industrial-scale preparation method of high-purity norbornene methyl silyl ether. The high purity monomers prepared according to the methods of the present invention can be used in a variety of applications, including but not limited to the preparation of high quality, high purity polynorbornene that can be used in a variety of electronics and other various applications.

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.

This invention provides an O,O'-monothiocarbonate compound and its preparation method, belonging to the field of organic chemical synthesis technology. This invention discloses a multi-component reaction of a silicon ether, elemental sulfur, and a difluorocarbene reagent under the action of an organic base to synthesize O,O'-monothiocarbonate compounds. Furthermore, the preparation method disclosed in this invention uses readily available and commercially available reactants, avoiding the use of hazardous and scarce reagents. The reaction conditions disclosed in this invention are mild, easy to operate, and yield a high quantity of O,O'-monothiocarbonates.

The invention provides a medetomidine preparation method, which comprises: S1, taking 2, 3-dimethyl benzaldehyde as an initial raw material, and carrying out a reaction on the 2, 3-dimethyl benzaldehyde and methylmagnesium chloride to generate 1-(2, 3-dimethyl phenyl) ethanol; s2, excessive silyl group protected imidazole is added into a reaction system in the step S1, and an activated [1-(2, 3-dimethylphenyl) ethyoxyl] silyl ether intermediate is obtained; taking trimethylsilyl trifluoromethanesulfonate as a catalyst, carrying out a Friedel-Crafts reaction with silyl-protected imidazole, and after the reaction is finished, carrying out post-treatment on the reaction liquid to obtain a medetomidine crude product. 2, 3-dimethyl benzaldehyde is adopted as a starting raw material, medetomidine is prepared through a one-pot method, raw materials are cheap, reaction steps are short, the production cost is greatly reduced, TMSOTf is adopted as a catalyst in the Friedel-Crafts reaction, the reaction is efficient, it can be effectively avoided that in the aftertreatment process of a traditional catalyst titanium tetrachloride, a large number of titanic acid colloidal solid insoluble substances are formed, and the yield of medetomidine is increased. The problem that post-treatment layering is difficult is solved, and the yield is increased.

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 composition comprises a silyl hydride, a silanol and / or a silyl ether, a Lewis acid catalyst, and a compound of the following formula: R 1 R 2 R 3 N [wherein the nitrogen is not a member of an N=CN bond, R 1 , R 2 , and R 3 wherein each of R is independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, and conjugated moieties; 1 , R 2 , and R 3 At least one of is a conjugated moiety connected to the nitrogen by a conjugated carbon.

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.

A process for the preparation of high purity norbornene alkyl silyl ether is disclosed and claimed. Specifically, a process for the preparation of industrial scale high purity norbornene methyl silyl ether is disclosed and claimed. The high purity monomers prepared in accordance with the process of this invention are useful in a variety of applications including but not limited to the preparation of high quality and high purity polynorbornenes having utility in a variety of electronic applications, among various other applications.

The embodiment of the invention provides a chromophore compound, a preparation method of the chromophore compound, an organic electro-optical material and application of the organic electro-optical material, and relates to the technical field of materials. The chromophore compound comprises a conjugate bridge, and a receptor and a donor which are respectively connected to two ends of the conjugate bridge through chemical bonds, the donor comprises aniline and a derivative structure thereof, and the aniline and the derivative structure thereof comprise silyl ether groups. By introducing the silyl ether group into the donor, the chemical stability and thermal stability of the chromophore compound can be improved. Meanwhile, when the chromophore compound is applied to the organic electro-optical material, the organic electro-optical material can have low dipole moment, and the nonlinear optical performance of the organic electro-optical material is improved. Furthermore, the donor in the chromophore compound has strong electron donating ability and can be cooperated with the receptor, and the beta value of the chromophore compound can be effectively improved, so that the organic electro-optical material can generate a larger electro-optical coefficient subsequently.

The present invention discloses a method for preparing a C-C bond coupling product from an enol silyl ether compound and the application of SF6, belonging to the technical field of organic photochemistry. In this method, an enol silyl ether compound and sulfur hexafluoride undergo a photochemical reaction at room temperature under the action of a light source and a photocatalyst to form a C-C bond coupling product; wherein the photocatalyst is N-phenylphenothiazine (PTH); and the light source is ultraviolet light with a wavelength of 365nm. Beneficial effects: This method utilizes sulfur hexafluoride to promote C-C bond coupling, and the reaction product is a 1,4-dicarbonyl compound that can be used in the synthesis and production of hybrid compounds such as pyrrole and furan; the reaction conditions are mild, and the raw materials are simple and readily available, thus having potential application value.

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 provides high-crystallinity heat-conducting polysulfate and a preparation method and application thereof, and belongs to the technical field of semiconductor materials.The preparation method comprises the steps that 4-cyanophenol and hydrazine hydrate are subjected to a heating reaction, and after the reaction is finished, washing and vacuum drying are conducted to prepare a first intermediate; adding the first intermediate into an ethanol solution, carrying out a heating reaction in an oxygen atmosphere, and after the reaction is finished, carrying out washing and vacuum drying to prepare a second intermediate; reacting the second intermediate with a silanizing agent, and purifying after the reaction is finished to obtain a monomer containing a silyl ether group; reacting the second intermediate with sulfuryl fluoride gas, and purifying after the reaction to obtain a monomer containing a sulfuryl fluoride group; and carrying out polymerization reaction on the monomer containing the silyl ether group or the second intermediate and the monomer containing the sulfuryl fluoride group to obtain the high-crystallinity polysulfate containing the tetrazine structure. The prepared high-crystallinity heat-conducting polysulfate is stable in physical and chemical properties, high in crystallinity and high in heat conductivity, and the preparation method is simple, efficient and low in cost.

A kudzuvine flower terpine derivative, a preparation method and application thereof, a structure formula is shown as follows: wherein R1, R2 are H, CH3, CH2F, CHF2, CF3, t-Bu, MOM, EE, THP, a straight chain or branched alkane with carbon atom number being 1-5, an ester group, a silyl ether, a trifluoro or polyfluorinated alkane straight chain terminal alkyne alkane n=1, 2, 3, 4 or 5, m=1, 2, 3, 4, 5 or 6, when one group is a terminal alkyne, the other two groups are alkane or fluorinated alkane. The kudzuvine flower terpine derivative can inhibit the proliferation growth of liver cancer cells, induce liver cancer cell apoptosis and G2 / M cycle arrest, inhibit the migration and invasion of liver cancer cells, achieve the effect of resisting tumors, and provide a new leading drug for clinical treatment of hepatocellular carcinoma.

The present application relates to the technical field of rubber synthesis, in particular to a kind of synthesis method of solution polymerized butadiene styrene.The synthesis method uses butadiene and styrene as monomer, cooperates double lithium chelate initiator, gradient polarity regulator and other raw materials, is prepared through polymerization, end-capping, coupling and post-processing step.Among them, double lithium chelate initiator is prepared by o-phenylenediamine silicon-based protection and lithiation reaction, contains stable five-membered chelate ring;Gradient polarity regulator is prepared by triethylene glycol through silylation and methylation, presents three-stage polarity gradient, and the controllability of polymerization is improved by the cooperation of the two.The synthesis method can accurately control the microstructure of the product, reduce ash content and volatile matter, improve mechanical properties and processing stability, and is suitable for the field of high-performance rubber products.

The present disclosure provides a compound having the structure of Formula (I): X-(Y)n-Z, wherein X is a drug comprising an anticancer agent; Y is a cleavable linker selected from esters, ethers, carbamates, amides, ketones, aldehydes, carboxylates, peroxides, anhydrides, amidines, hydrazones, imines, imides, azides, cyanates, nitriles, thiols, sulfides, sulfoxides, sulfones, thiocyanates, thials, thioesters, phosphonic acids, phosphodiesters, boronic acids, and silyl ethers; and Z is a carborane isomer comprising ortho-, meta-, or para-carborane; or a pharmaceutically acceptable salt or solvate thereof. The disclosure also provides methods of treating cancer using the compound and pharmaceutical compositions comprising the compound and a pharmaceutically acceptable excipient.

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.