6 results about "Trimethyl orthoformate" patented technology

The application provides a preparation method of 3-aryl / alkyl-beta-naphthyl ether compounds, and the preparation method comprises the following steps: reacting trimethyl orthoformate with 1,3-diaromatic propyl ketone compounds or 1-aryl-3-alkyl ketone compounds to obtain 3-aryl-beta-naphthyl ether compounds or 3-alkyl-beta-naphthyl ether compounds. The reaction condition of the application is mild, trimethyl orthoformate is cheap and easy to obtain, can be used as a methylation reagent and a carbon source for extending a carbon chain at the same time, the range of reaction substrates is wide, and the functional group tolerance is good; the reaction is efficient, the selectivity is high, the post-treatment is simple, the operation is simple, and the application is suitable for large-scale industrial production; the complex substrate prepared in advance in the traditional reaction is avoided, the metal catalyst necessary for the traditional reaction is not needed, the binaftyl alcohol precursor compounds can be prepared with high chemical selectivity, and a more simple and efficient route is provided for the olefin hydroformylation / hydroformyl esterification reaction for synthesizing bidentate ligands.

The application discloses a preparation method of a nanofiber-based flame-retardant functionalized diaphragm and a lithium battery. The preparation method comprises the following steps: adding polyacrylonitrile into N,N-dimethylformamide and stirring until the PAN is completely dissolved to obtain a spinning precursor solution; performing electrostatic spinning on the spinning precursor solution to obtain a PAN nanofiber membrane; dropping trimethyl orthoformate into trifluoromethanesulfonic anhydride to obtain a first mixed solution; soaking the PAN nanofiber membrane in the first mixed solution and stirring and soaking; adding a second mixed solution composed of diethyl phosphite and dichloromethane into the first mixed solution, stirring and soaking and reacting to obtain the nanofiber-based flame-retardant functionalized diaphragm. The prepared phosphate-based functionalized PAN diaphragm has good flame retardancy and can be self-extinguished rapidly when contacting a flame; has high heat resistance and still maintains good fiber morphology at 200 DEG C; exhibits a high electrochemical stability window, so that the diaphragm also shows excellent application potential in high-voltage-resistant batteries.

The present application relates to a kind of preparation methods of 3,4-dihydroxy-5-methoxybenzoic acid methyl ester, with gallic acid as raw material, it is reacted with trimethyl orthoformate or trimethyl orthoacetate, trimethyl orthoformate or trimethyl orthoacetate can realize the protection of adjacent diphenol hydroxyl on one hand, on the other hand, carboxyl esterification and 5-hydroxyl are methylated, form the methyl ester of 5-phenolic hydroxyl methylation and 3,4-orthoester protection benzoic acid shown in formula 1a or formula 1b, further by acidic solution treatment, deprotection is carried out, and the target product 3,4-dihydroxy-5-methoxybenzoic acid methyl ester is prepared.The preparation method is mild in reaction condition, process is simple, easy to operate, product yield and purity are high, solve the wastewater problem in borax protection method, and avoid using toxic dimethyl sulfate for methylation, process condition is simple, easy to operate, convenient for industrialization, with very high application value.

A scale-up preparation method for 4-(dimethoxymethyl-4-piperidine)phenylboronic acid pinacol ester, relating to the technical field of pharmaceutical intermediates. The method comprises: using 4-piperidinecarboxaldehyde as a raw material to react with a sulfite and protecting an aldehyde group to obtain intermediate A; then performing a coupling reaction with potassium 4-boronic acid pinacol ester phenyltrifluoroborate to generate intermediate B; then performing deprotection on the intermediate B in the presence of an inorganic base to obtain intermediate C; and finally reacting the intermediate C in the presence of trimethyl orthoformate to obtain 4-(dimethoxymethyl-4-piperidine)phenylboronic acid pinacol ester. The method significantly reduces reaction steps, reduces raw material costs, has a simple and reliable process, is suitable for industrial production, and provides a new reaction route for product synthesis.

The invention relates to a synthesis method of an azoxystrobin intermediate, and belongs to the technical field of organic synthesis.The synthesis method comprises the steps that benzofuranone serves as a raw material and is directly condensed with formate under the action of alkali, then dimethyl sulfate is methylated, and 3-(alpha-methoxyl) methylene benzofuranone is obtained. The use of expensive trimethyl orthoformate is avoided, and the cheap and easily available formate is adopted, so that the raw material cost of the azoxystrobin intermediate is greatly reduced, and the method is simple in process route, high in yield and suitable for industrial production.

The invention provides a preparation method of a zavazepam intermediate 3-(piperidine-4-yl)-1, 2-dihydroquinoline-2-ketone or a salt of the zavazepam intermediate 3-(piperidine-4-yl)-1, 2-dihydroquinoline-2-ketone. The preparation method comprises the following steps: by taking tert-butyl bromoacetate and trimethyl orthoformate as raw materials, carrying out condensation to obtain 2-bromoalkene tert-butyl propionate, then carrying out Suzuki coupling on the 2-bromoalkene tert-butyl propionate and N-tert-butyloxycarboryl piperidine-4-boronic acid pinacol ester to obtain 2-(N-tert-butyloxycarboryl piperidine-4-yl) tert-butyl acrylate, and then hydrolyzing the 2-(N-tert-butyloxycarboryl piperidine-4-yl) tert-butyl acrylate to obtain an acrylic acid derivative. The preparation method comprises the following steps: directly constructing a quinoline-2-ketone core skeleton by coupling-cyclizing acrylic acid and 2-bromoaniline through a one-pot method in the presence of palladium catalysis and a dehydrating agent to obtain a Boc protection intermediate, and finally performing acidolysis deprotection to obtain a target product. The route thoroughly avoids sodium hydride, LDA, iron powder and other dangerous or high-pollution reagents, conditions are mild, operation is safe, three wastes are few, all intermediates and products can be purified through conventional crystallization, column chromatography is not needed, the total yield is high, and the method is suitable for industrial production.