9 results about "Triethylsilane" patented technology

The present invention relates to the technical field of organic synthesis, and specifically relates to a method for constructing the chirality of a pyran ring in Orforglipron by means of enzymatic catalysis, the method comprising the following steps: step S1, by using SM1 and SM2 as starting materials, carrying out a reaction under the action of a palladium catalyst and a ligand to obtain INT-1; step S2, under the catalysis of Pd / C, subjecting INT-1 to double bond hydrogenation reduction to obtain INT-2; step S3, in the presence of a solvent, a buffer salt system and enzymatic catalysis, subjecting INT-2 to hydrolysis and resolution to obtain a chirally pure intermediate INT-3; step S4, subjecting INT-3 to a Grignard reaction for cyclization, so as to synthesize a lactone intermediate INT-4; and step S5, subjecting INT-4 to reduction by means of Dibal-H, quenching same, performing extraction with dichloromethane, drying same with anhydrous sodium sulfate, and then performing reduction by means of triethylsilane to obtain a compound of general formula A. In the present invention, the chirality is constructed by means of enzymatic catalysis without the need of SFC resolution for separating isomeric impurities during the construction of the chirality, thereby reducing losses and improving yield, obtaining the target product at high yield and high chiral selectivity, and further saving expenses and reducing costs.

The invention relates to the technical field of organic synthesis, in particular to a method for continuously producing canagliflozin by using a microchannel reactor. The production method comprises the following steps: reacting M1 and isopropyl magnesium chloride lithium chloride in a microreactor 1 to form an intermediate I; the reaction temperature is-10 DEG C to 10 DEG C; the reaction time is 15 to 45 seconds; reacting the intermediate I with the M2 in a microreactor 2 to form an intermediate II; the reaction time is 20 to 60 seconds; reacting the intermediate II, methanesulfonic acid and C1-C3 alcoholic solution in a microreactor 3 to form an intermediate III; the reaction time is 20 to 60 seconds; and reacting the intermediate III, triethyl silane and boron trifluoride diethyl etherate in a microreactor 4 for 5-10 seconds. The method solves the problems that the micro-channel reactor is easy to block and the product purity is not high.

The invention discloses a synthesis method of high-purity triethyl silane, and belongs to the technical field of organosilicon compound synthesis. The method solves the problems of low purity, poor stability and serious pollution of the existing synthesis method, sodium hydride and trimethyl borate are used as starting raw materials, a trimethoxy sodium borohydride solution is generated in situ under a low-temperature condition, then the trimethoxy sodium borohydride solution and accurately metered triethyl chlorosilane are subjected to a mild and controllable reduction reaction, and the high-purity triethyl chlorosilane is obtained. According to the method, the dependence of a traditional process on a noble metal catalyst or a highly toxic reducing agent is abandoned, the reaction safety is improved from the source, the complete reaction is promoted by adopting the composite catalyst, and the hydrophobic modified 3A molecular sieve is innovatively utilized for low-temperature adsorption purification, so that key impurities such as trace moisture and chloride ions can be efficiently removed; and finally, high-vacuum precise rectification is combined, so that a high-purity triethyl silane product can be obtained.

The application relates to the technical field of compound synthesis, and discloses an aromatic dipeptide functionalized mercapto compound, 3,5-di(triphenylmethylthio)benzoic acid is obtained by adding 3,5-di(methylmercapto)benzoic acid and pyridine into a solution of chloromethyl triphenylphosphonium, purifying after sufficient reaction; then the 3,5-di(triphenylmethylthio)benzoic acid is mixed with N-hydroxysuccinimide and dissolved in an organic solvent, EDC.HCl is added, purifying after sufficient reaction; then 2,5-dioxopyrrolidin-1-yl 3,5-bis(triphenylmethylthiomethyl)benzoate is obtained; then phenylalanine-tryptophan and triethylamine are added, purifying after sufficient reaction; then (3,5-bis(triphenylmethylthiomethyl)benzoyl)tryptophylphenylalanine is obtained; then trifluoroacetic acid and triethylsilane are added, purifying after sufficient reaction; and finally the aromatic dipeptide functionalized mercapto compound is obtained. The aromatic dipeptide functionalized mercapto compound can quickly and effectively identify sodium and potassium ions, and has relatively low detection limit and relatively loose detection condition.

The invention discloses a preparation method of fulvestrant, according to the preparation method, triphenyl halogenated methane is used as a hydroxyl protection reagent, more target products are generated during alkyl chain substitution through a steric effect, in addition, triethyl silane and boron trifluoride diethyl etherate are used for reducing carbonyl and removing protection at the same time, and the reaction conditions are simple and mild. Meanwhile, carbonyl and protecting groups are removed in the step, so that subsequent thioether bonds are not affected, the impurity amount is reduced, raw materials in the whole reaction route are cheap and easy to obtain, the preparation route is short, the overall molar yield reaches 65%, and a reference route is provided for industrial preparation of fulvestrant.

This utility model relates to the field of triethylsilane synthesis technology and discloses an apparatus for triethylsilane synthesis, comprising: a raw material storage component for storing synthesis raw materials; a mixing device for mixing the raw materials output from the raw material storage component; and a fixed-bed reactor filled with a catalyst. By providing the temperature required for the reaction, the mixed raw materials react with each other on the catalyst surface under certain pressure and temperature to generate the desired substance. This utility model provides a production apparatus for triethylsilane, which is a fully continuous process device including reaction and separation processes. This apparatus supports the production of triethylsilane from tetrahydrosilane and ethylene via fixed-bed catalytic reaction. The apparatus has a simple process, high atom utilization, simplified flow, no solvent use, low waste, and can achieve continuous and automated operation.

This invention relates to the field of asymmetric catalytic hydrogenation, specifically to a method for preparing chiral chromone or chromane carboxylic acid compounds. The method involves preparing a chiral catalyst from a nickel compound and ligands. By controlling the combination of the nickel compound-ligand-solvent, enantioselective hydrogenation of the conjugated C=C bonds of the substrate chromone carboxylic acid compound is achieved, yielding the semi-reduced product chiral chromone carboxylic acid; or, further, the carbonyl group is reduced, and carbonyl reduction and dehydroxylation reactions are carried out at room temperature under trifluoroacetic acid and triethylsilane conditions to obtain the fully reduced product chiral chromane carboxylic acid. The catalytic system of this invention is simple to construct, and the selectivity can be controlled by the solvent system. It maintains high conversion and excellent enantioselectivity even under high S / C conditions, making it suitable for the efficient preparation of chiral chromone / chromane skeletal carboxylic acid compounds.

The invention provides an alkyl uracil derivative and a preparation method and application thereof, and relates to the technical field of organic synthesis.The preparation method comprises the following steps that a uracil analogue and olefin are subjected to a hydrogenation alkylation reaction under the action of an iron catalyst and a hydrogen source, and the alkyl uracil derivative is obtained; the iron catalyst comprises at least one of iron nitrate nonahydrate, ferrous nitrate, ferric chloride, ferrous chloride, ferric sulfate and ferric oxalate; the hydrogen source comprises at least one of sodium borohydride, lithium borohydride, lithium aluminum hydride, triphenyl silicon, triethyl silicon and borane. According to the present invention, the olefin is adopted as the alkyl raw material, the pre-functionalization is not required, the specific catalyst and the specific hydrogen source are combined, the hydrogenation alkylation reaction of the olefin and the uracil analogue is successfully achieved, and the technical effect of constructing a series of alkyl uracil derivatives is achieved. According to the invention, the reaction can be carried out at room temperature without light and heat conditions, the reaction time is short, and the functional group tolerance is better.

The invention discloses a novel synthesis method of 5-aryl-3-alkyl pyrazolo [1, 5-a] pyridine, which comprises the following specific synthesis steps: adding an X2 donor compound into a solvent containing a compound SM at 0-5 DEG C, stirring at 0-5 DEG C for complete reaction, and performing post-treatment to obtain a compound 1; adding the compound 1 into a solvent, adding an organic metal reagent at 0-5 DEG C in a protective atmosphere, stirring at room temperature for complete reaction, and performing post-treatment to obtain a compound 2; dissolving the compound 2 and triethyl silane in a solvent, adding trifluoroacetic acid, stirring to react completely, and performing post-treatment to obtain a compound 3; under a protective atmosphere, dissolving the compound 3, Pd (dppf) Cl2, B2Pin2 and alkali in an organic solvent, and carrying out reflux stirring reaction completely to obtain a compound 4; and under a protective atmosphere, adding water, Pd (dppf) Cl2 and ArX into the reaction liquid containing the compound 4, carrying out reflux stirring to completely react, and carrying out post-treatment on the reaction liquid to obtain a target compound 5. The method is short in step, easy to operate in each step, high in yield and suitable for large-scale amplification.