71 results about "Tert-butyldimethylsilyl chloride" patented technology

The invention relates to a preparation method and application of a double-photon fluorine ion fluorescent probe compound. The formula of the double-photon fluorine ion fluorescent probe compound is as shown in formula I. The preparation method includes: allowing 2, 4-dihydroxy benzaldehyde and cyclohexenone to react under nitrogen protection by using imidazole as the catalyst; allowing the product obtained by separation to react with tert-butyldimethylsilyl chloride to obtain the pure fluorine ion fluorescent probe compound. The fluorine ion fluorescent probe compound has the advantages that the probe compound has good selectivity and sensitivity to fluorine ions and is nontoxic to cells; probe molecules can be stimulated by double photons to avoid an ultraviolet region, so that the probe molecules are applicable to detection of the fluorine ions in water and detection and imaging of the fluorine ions in cells.

The invention discloses a preparation method for cytidine. The method includes following steps: firstly, subjecting cytosine to silanization protection by tert-butyl dimethyl chloro silane; secondly, reacting with tetra-o-acetyl-d-ribose; thirdly, obtaining crude cytidine by ammonolysis of the reactant; and fourthly, adding the crude cytidine to ethanol for refinement, heating, refluxing and dissolving while stirring and adding water, devitrifying after cooling, separating to obtain solid, and drying to obtain the cytidine. The preparation method for the cytidine is simple in process route, low in cost, low in environmental pollution and safe in production, is a route suitable for industrial production and has wide application prospect.

The invention discloses a preparation method of a Dapagliflozin intermediate used for treating II-type diabetes. The preparation method comprises the following steps: 1) performing a reaction on 5-bromine-2-chlorobenzoic acid and oxalyl chloride in anhydrous dichloromethane under the catalysis of DMF (dimethyl formamide), so as to obtain 5-bromine-2-chloro-benzoyl chloride; 2) under the condition that tert-Butyldimethylsilyl chloride exists, performing a reaction on 5-bromine-2-chloro-benzoyl chloride obtained in step 1) and phenetole under the catalysis of ferric trichloride, so as to obtain 5-bromine-2-chloro-4'-ethyoxyl benzophenone. According to the preparation method provided by the invention, no ortho-by-product is generated, and the yield of a target product is high, so that the good support of storage of raw materials is provided for Dapagliflozin. Additionally, the preparation method is mild in conditions and short in reaction time, therefore, the preparation method is suitable for industrial production and promotion.

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 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.

The invention discloses a modified activated carbon adsorbent for adsorbing and removing refractory organics. Activated carbon is cleaned and then modified with mixed liquid prepared from NbCl4, ZnCl2, Cu(NO3)2 and Mg(NO3)2 to obtain matter B; the matter B is modified with mixed liquid prepared from sodium aluminate, ammonium hexafluorophosphate, potassium borohydride and lithium chloride to obtain matter D; the matter D is modified with mixed liquid prepared from tert-butyldimethylsilyl chloride, cyclohexanecarboxaldehyde, phenyltrimethoxysilane, 2,2,3,3-tetrafluoropropyl 4-toluenesulfonate and hydroxypropyl-beta-cyclodextrin to obtain matter which is the modified activated carbon adsorbent for adsorbing and removing the refractory organics. The prepared modified activated carbon adsorbent has the advantages that for the refractory organics in waste water, the adsorbing efficiency is high, and the adsorption capacity is large.

The invention relates to the field of a film, and specifically speaking relates to a composition used for preparing an anti-corrosion heat-insulation automobile film and a preparation method thereof.An anti-corrosive coating employs butyl 4-hydroxybenzoate as a main raw material to increase the anticorrosion performance of the automobile film, tert-butyldimethylsilyl chloride is used for protecting a hydroxyl group in butyl 4-hydroxybenzoate, stability of butyl 4-hydroxybenzoate is effectively increased, acid-resistant performance is increased, a preferably selected anti-oxidant is combined with poly-L-monosodium glutamate for usage, and stability effect can be achieved. through preferably selecting the usage materials of a thermal-insulation layer and a wearing layer, and the heat insulation and antifriction effects are better than that of the prior art. An improved copolymer and carboxyl-terminated hyperbranched polyester are employed, so that long-term storage is achieved, and theperformance cannot be changed.

The invention discloses a synthetic method of a polyhydroxy marine steroid (25R)-5 Alpha- cholest-2 Beta and a 3 Alpha and 26-triol, which uses a low-cost Tigogenin as the raw material and obtains (25R)-5 Alpha-cholest-2-ene-16 Beta and 26-diol through the TsCl esterification, elimination reaction and the reduction of zinc powder/ethanol system, obtains (25R)-26-O- t butyl dimethysilyl-5 Alpha- cholest-2-ene through selectively protecting C-26- hydroxyl, C-16-hydroxyl ethlsulphonic acid esterification and lithium aluminum hydride reduction by t-butyl dimethylsilyl chloride, and at last gets the object compound (25R)-5 Alpha- cholest-2 Beta, 3 Alpha and 26-triol through ring-opening under the acid conditions after the epoxidation. The synthetic route of the invention is characterized in that: the synthetic raw material is of low-cost and easy to get; the synthetic route is scientific and reasonable, etc. The target compound has potential antitumor and antivirus activity.

The invention belongs to the technical field of chemistry and medicine, and discloses an efficient total synthesis method and application of a natural product schaftoside. The method comprises the steps of subjecting naringenin, tert-butyldimethylsilyl chloride and acetyl chloride to reaction to obtain an intermediate compound 2, and conducting deoxidation reaction to obtain an intermediate compound 3; carrying out rearrangement reaction on the intermediate compound 3 to obtain an intermediate compound 5, and removing a silicon-based protecting group to obtain an intermediate compound 6; carrying out rearrangement reaction on the intermediate compound 6 to obtain an intermediate compound 8; reacting the intermediate compound 8 with benzyl bromide in potassium carbonate to obtain an intermediate compound 9; oxidizing the intermediate compound 9 by ceric ammonium nitrate and pyridinium dichromate to obtain an intermediate compound 10; removing benzyl from the intermediate compound 10 to obtain an intermediate compound 11; and catalyzing the intermediate compound 11 to obtain an intermediate compound 12, and removing acetyl to obtain a target product compound. The method is mild in reaction condition, convenient to operate, economical in raw materials and capable of being used for industrial preparation.

The present invention provides a synthesis method for increasing ginsenoside M1 and decanoylchloride monoesterification selectivity. According to the synthesis method, the hydroxyl at the site 6 of the ginsenoside M1 glycoside group is protected by using tert-butyldimethylsilyl chloride through an etherification manner, the obtained material and equivalent decanoylchloride are subjected to a monoesterification reaction in an ice water bath under nitrogen protection by adopting dichloromethane as a solvent and adopting triethylamine as an acid binding agent under a DMAP (4-dimethylaminopyridine) catalysis condition, and finally tetrabutylammonium fluoride is adopted to remove the silicon-protected group to obtain the product of the monoesterification reaction of the tert-butyldimethyl siloxane of the ginsenoside M1 and the decanoylchloride.

The invention discloses a sealing strip for a cab instrument desk. The sealing strip comprises the following raw materials in parts by weight: 20-50 parts of butadiene styrene rubber, 2-8 parts of tert-butyldimethylsilyl chloride, 5-12 parts of chlorosulfonated polyethylene, 1.5-3.5 parts of a cross-linking agent, 30-50 parts of a black mica compound, 5-15 parts of vermiculite power, 20-30 parts of talcum powder, 2-10 parts of expanded perlite, 2-8 parts of a multi-walled carbon nano tube, 3.5-4.5 parts of a compatilizer, 1-2 parts of ethylene glycol dimethacrylate, 0.5-1.5 parts of hydroquinone, 1-2 parts of p-phenylenediamine and 2-3 parts of magnesium stearate. The sealing strip for the cab instrument desk has excellent high temperature resistance, anti-aging property, excellent sealing effect, promoted comfortable sensation of the passenger, difficulty in falling off, easily available raw materials and low cost.

The invention discloses a preparation method for a rosuvastatin calcium intermediate. The preparation method comprises the following steps: adding Salen Co (III) in a sodium acetylide tetrahydrofuran solution, dropwise adding epichlorohydrin for reaction, dropwise adding a product into a sodium cyanide aqueous solution for reaction to obtain a product, and dropwise adding the obtained product into methanol and introducing hydrogen chloride to obtain (3R)-hydroxyl-methyl 5-octynoate (III); with dichloromethane as a solvent, adding the compound (III) and tert-butyldimethylsilyl chloride to obtain a compound (IV), dropwise adding the compound (IV) into a sodium hypochlorite aqueous solution to obtain 6-chloro-(R)-(+)-3-(tert-butyldimethylsilanyloxy)-5-oxo-methyl caproate (V); with 2-methyltetrahydrofuran as a solvent, adding 6-chloro-(R)-(+)-3-(tert-butyldimethylsilanyloxy)-5-oxo-methyl caproate and triphenylphosphine so as to obtain methyl (3R)-(tert-butyldimethylsilanyloxy)-5-oxo-6-triphenylphosphoranylidenehexanoate(VI). According to the preparation method provided by the invention, the raw materials are simple, the reaction conditions are mild, environment friendliness is realized and the preparation method can be used for industrial mass production.

The invention relates to a method for preparing tert-butyldimethyl chlorosilane, which is characterized by comprising the following steps of: a, in a synthesis kettle, putting 10 to 15 weight parts of magnesium into 160 to 240 volume parts of mixed solvent consisting of ether and cyclohexane, dripping mixed solution consisting of 35 to 55 weight parts of tertiary butyl chloride and 50 to 78 weight parts of dimethyl dichlorosilane into the mixed solvent at the temperature of between 40 and 55 DEG C, a preserving heat for 2.5 to 3.5 hours after the dripping is finished to obtain a synthesized material; b, transferring the synthesized material to a dissolution kettle, cooling the synthesized material to between 10 and 15 DEG C, then dripping 400 to 600 volume parts of 25 to 30 percent hydrochloric acid into the dissolution kettle, standing and demixing the solution, and removing wastewater at the bottom to obtain upper liquor; and c, transferring the upper liquor in the dissolution kettle to a rectification kettle to perform purification, and removing the solvent to obtain a tert-butyldimethyl chlorosilane product. The method has the advantages of simple synthesis process, high safety and stable product yield.

Relating to the technical field of paint, the invention provides a laptop case paint coating and a preparation method thereof. The laptop case paint coating is prepared from the following raw materials: polyurethane, n-butanol, an amino-silane coupling agent, p-xylene, tert-butyldimethylsilyl chloride, cognac oil, tributyl tin methacrylate, spherical silver powder, gamma-Nonanolactone, epoxy resin, triruthenium dodecacarbonyl, alumina particles, bentonite and deionized water. The preparation method consists of: mixing the amino-silane coupling agent, p-xylene, tert-butyldimethylsilyl chloride, spherical silver powder and triruthenium dodecacarbonyl evenly, then performing standing, adding gamma-Nonanolactone and epoxy resin, stirring the substances evenly, and then conducting high-speed shearing; b. mixing polyurethane and n-butanol and carrying out stirring reaction, then adding cognac oil, tributyl tin methacrylate, bentonite, alumina particles and deionized water and performing mixing; and c. adding the raw material obtained in step a into the product of step b, and carrying out high-speed shearing and static cooling. The laptop case paint coating provided by the invention has the characteristics of good wear resistance, good flame resistance, high strength, and difficult discoloration and shedding.

The invention discloses a method for preparing an intelligence-improving medicine (S)-oxiracetam. The method comprises the following steps: (1) under the catalysis of 4-dimethylaminopyridine, enabling 2-oxiraneisobutylacetate to contact with ammonia gas to react, so as to obtain (S)-4-hydroxyl-2-oxopyrrolidine; (2) enabling the (S)-4-hydroxyl-2-oxopyrrolidine obtained by the step (1) to react with tert-butyldimethylsilyl chloride, so as to obtain a compound shown as a formula III, which is protected by tert-butyl dimethylsilane; (3) enabling the compound shown as the formula III and 2-bromoacetic ester to be subjected to a nucleophilic reaction under an alkaline condition, so as to obtain a compound shown as a formula IV; (4) under the catalysis of ammonium chloride, enabling the compound shown as the formula IV and ammonia gas to be subjected to an ammonolysis reaction, so as to obtain the (S)-oxiracetam as shown in the description. The (S)-oxiracetam prepared by the method provided by the invention is high in yield, high in ee value and relatively low in cost, and a preparation process is simple and is suitable for industrial production.

The invention discloses a synthesis method of 2-bromo-5-methoxyphenol. According to the synthesis method, 3-methoxyphenol is taken as a raw material, firstly, the 3-methoxyphenol reacts with a protection reagent such as tert-butyldimethylsilyl chloride, acetyl chloride, acetic acid and acetic anhydride, and then hydroxide radicals are protected; then an obtained intermediate is subjected to a bromination reaction; finally, an obtained bromination product is de-protected to obtain the 2-bromo-5-methoxyphenol. The method has the advantages that the operation condition is mild and safe, aftertreatment is simple, and the conversion rate is high. The yield achieved by means of the synthesis method is far higher than that of an existing direct bromination method, and aftertreatment is relativelysimple.

The invention relates to the technical field of auto films, in particular to an ultraviolet-resistant corrosion-resistant auto film and a preparation method thereof. The auto film mainly contains polymethyl methacrylate, poly diisooctyl phthalate, propylene glycol p-toluate, tert-butyldimethylchlorosilane, phosphate ester emulsifier, low methyl etherified melamine formaldehyde resin, diisooctyl phthalate, sodium metabisulfite, molybdenum dialkyldithiocarbamate and ultraviolet-resistant nanocomposite. The prepared auto film is good in ultraviolet absorption, high in transmittance, resistant toacid and alkali corrosion, simple in preparation process and suitable for mass production.

The invention discloses a novel preparation method of calcipotriol. According to the preparation method, stigmasterol-2 is adopted as a starting material, alpha hydroxyl and tert-butyldimethylsilyl chloride are introduced in through microbial fermentation for carrying out seven steps of reactions including hydroxy protection, O3 oxidation, witting reaction, reduction, illumination isomerization, deprotection of hydroxys, and the like, so as to obtain calcipotriol.

A methanol gasoline rubber swelling inhibitor is prepared from the following ingredients in parts by weight: 12 parts of 2-mercaptobenzothiazole, 8 parts of iodopropynyl butylcarbamate, 1 part of butylated hydroxyanisole, 16 parts of 2,6-butylated hydroxytoluene, 8 parts of sodium dodecyl sulfonate, 13 parts of 2-ethylimidazole, 6 parts of dichloro[(1,2,5,6-eta)-cycloocta-1,5-diene]ruthenium, 9 parts of methoxypropiophenone, 2 parts of polyisobutylene succinimide, 3 parts of tert-butyldimethylsilyl chloride and 12 parts of methyl tert-butyl ether. The methanol gasoline rubber swelling inhibitor is used by the method that the methanol gasoline rubber swelling inhibitor is directly added into methanol gasoline M15-M30 and mixed uniformly, and the adding quantity is 0.4-0.7% of the weight of the methanol gasoline. The methanol gasoline rubber swelling inhibitor has excellent oxidation resistance and excellent corrosion resistance, and can prevent related seal parts of a vehicle from being worn or corroded, keep the elasticity of rubber components and prevent rubber aging.

The invention discloses an outdoor valve sealing gasket in a southern region. The outdoor valve sealing gasket comprises the following raw materials in parts by weight: 75-85 parts of chloroprene rubber, 25-45 parts of chlorosulphonated polyethylene, 20-30 parts of fluorinated silicone rubber, 4-8 parts of a polytetrafluoroethylene degradation complex, 60-80 parts of a filling reinforcing agent, 1.5-2.5 parts of tert-butyldimethylsilyl chloride, 1-2 parts of disproportionated rosin, 1-2 parts of hydroxyl silicone oil, 2-4 parts of a cross-linking agent, 1.5-3.5 parts of an ultraviolet absorberand 2-4 parts of an antioxidant BHT. The polytetrafluoroethylene degradation complex is prepared by the following process steps: performing irradiation-induced degradation on the polytetrafluoroethylene resin, exhausting air and degassing, grinding, adding collagens, keratin and water to be uniformly mixed, regulating the pH value of the system to be 6.1-6.5, stirring, filtering, washing, and drying, thereby obtaining the polytetrafluoroethylene degradation complex.

The invention discloses a novel synthesis method for a key intermediate of the anti-hepatitis B drug Entecavir. The method is characterized in that a known compound as shown by Formula 1 is adopted asa starting material, and synthesis of target molecules is achieved through a series of reaction steps such as Evans aldol reaction, hydroxyl protection through tert-butyldimethylsilyl chloride, reductive removal of a chiral auxiliary group through diisobutyl aluminum hydride (DIBAL-H) to obtain an aldehyde, addition of a Grignard reagent into the aldehyde, protection of a newly generated hydroxylthrough tert-butyldimethylsilyl, double-bond epoxidation reaction, free-radical ring closing reaction, hydroxyl protection through p-methoxybenzyl, etc. The method disclosed by the invention has theadvantages of unique and novel designing of the whole route, mild reaction conditions for the reaction steps, high rate, relatively fewer side effects, and high simplicity and convenience in operation; and common chemical reagents are adopted in the route, and raw materials are cheap and can be easily obtained, so that the synthesis cost can be greatly reduced.

The invention discloses a monomer for polymer gel, the polymer gel and a preparation method. The preparation method comprises the following steps of: reacting 4, 4', 4''-trihydroxytriphenylmethane with tert-butyldimethylsilyl chloride to obtain TPC-OTBS; reacting 4, 4', 4''-trihydroxy triphenylmethane with sulfuryl fluoride in the presence of triethylamine to prepare TPC-OSO2F; and dissolving TPC-OTBS and TPC-OSO2F in DMF, adding DBU, carrying out uniform ultrasonic dispersion, and standing to obtain the polymer gel. The gel obtained by the invention can selectively adsorb an organic solvent through electrostatic interaction and Van der Waals force. SEM (scanning electron microscope) and TEM (transmission electron microscope) are used for characterizing the surface and internal morphology of a solid material, the porous morphology of the solid material is found, and pores are most macropores. The structure of cross-linked polysulfate is represented by infrared and nuclear magnetism, a solid nuclear magnetism fluorine spectrum and an XPS element prove that a monomer sulfonyl fluoride group is completely reacted, and the polymer gel has a better application prospect in the aspect of adsorption due to the interaction force between the cross-linked polysulfate and a solvent.

The invention introduces a synthetic method for improving ginsenoside M1 and iso-butyryl chloride mono-esterification selectivity. Firstly, No.6 hydroxy of glycosyl of ginsenoside M1 is protected by using tert-butyldimethylsilyl chloride through esterification, and is subjected to mono-esterification reaction with equivalent iso-butyryl chloride in the ice-water bath under the nitrogen protection with dichloromethane as a solvent and triethylamine as an acid applying agent under the DMAP (4-dimethylamino-pyridine) catalysis; finally, a silicon protecting group is removed by using tetrabutylammonium fluoride.

The present invention provides a method for preparing epirubicin and an intermediate adaptive to the method. The preparation method may include: reacting tert-Butyldimethylsilyl chloride with N-trifluoroacetyl adriamycin to obtain a first compound N-trifluoroacetyl-14-O-tert-Butyldimethylsilyl adriamycin; oxidizing the first compound to obtain a second compound 4′-ketone-N-trifluoroacetyl-14-O-tert-Butyldimethylsilyladriamycin; reducing the second compound to obtain a third compound N-trifluoroacetyl-14-O-tert-Butyldimethylsilyl epirubicin; and performing deprotection and hydrolysis reactions on the third compound to obtain epirubicin. The method of the present invention needs low cost, fewer reaction steps, provides high yield and high product purity, and avoids serious pollution caused by a bromination reaction in a conventional method.

The invention discloses a preparation method of p-phenylenebenzobisoxazole-silsesquioxane copolymer, which utilizes tert-butyldimethylchlorosilane to treat easily oxidized and poorly soluble 4,6-diaminomethylene Active amino groups and hydroxyl groups in quinone dihydrochloride monomers are chemically modified to obtain monomers protected by silane functional groups, increasing their solubility and stability in organic solvents; at the same time, using terephthaloyl chloride and The acylation reaction of the two hydroxyl POSS makes the terminal active hydroxyl group containing the regular cage structure POSS be converted into an acid chloride group; finally, the monomer protected by the silane functional group and the terminal acylated POSS and terephthaloyl chloride are dissolved in an organic solvent The polycondensation reaction is carried out, and the cage structure POSS monomer is chemically bonded to the PBO main chain by chemical methods to obtain a block copolymer. The block copolymer prepared by the invention has good solubility and film-forming property, and has excellent high temperature resistance and mechanical properties.