12 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 invention belongs to the technical field of drug synthesis, and particularly relates to a method for preparing a high-purity butrol lithium complex. The preparation method of the present invention comprises the following steps: (1) 9-fluorenone and trimethyl orthoformate are activated by iron p-toluenesulfonate to obtain a ketal, the ketal and cis-1,4-diol are exchanged to obtain a cyclic ketal, and the cyclic ketal is oxidized to obtain an epoxy side chain 3,5,8-trioxaspiro[bicyclo[5.1.0]octane-4,9'-fluorene]; (2) cyclocyclohexane and 3,5,8-trioxaspiro[bicyclo[5.1.0]octane-4,9'-fluorene] are subjected to an epoxy ring-opening reaction in an organic solvent under the action of a lithium salt to generate an intermediate I; (3) the intermediate I and an α-substituted acetate are subjected to nitrogen alkylation in an organic solvent to generate an intermediate II; (4) the ester group of the intermediate II is hydrolyzed under alkaline conditions to obtain an intermediate III; and (5) the ketal is removed from the intermediate III under acidic conditions to obtain a butrol lithium complex.

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 embodiment of the invention discloses a preparation method of 1-butene-3, 4-diol, which comprises the following step of: reacting erythritol with trimethyl orthoformate under the action of a rhenium catalyst, organic acid and a polymerization inhibitor to obtain the 1-butene-3, 4-diol. According to the embodiment of the invention, the effects of simple steps, cheap and easily available raw materials, good catalyst selectivity, recycling, environment friendliness, low cost and easiness in industrial production are realized.

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.

The application discloses a method for synthesizing ultraviolet absorber in the technical field of ultraviolet absorber, and the method comprises the following steps: taking 50g of SAPO-5 zeolite molecular sieve, and activating the SAPO-5 zeolite molecular sieve with 1000ml of sulfuric acid with a concentration of 0.001M, 1000ml of glacial acetic acid and 1000ml of propionic acid respectively at room temperature for 30min; washing and drying: after the activation is completed, the SAPO-5 zeolite molecular sieve catalyst is obtained by centrifugal washing with deionized water and drying at 80 DEG C for 12h; N-methylaniline, trimethyl orthoformate, ethyl p-aminobenzoate and the catalyst obtained in step S2 are weighed and mixed according to a proportion to obtain a mixed solution; the mixed solution obtained in step S3 is placed in a three-necked flask, the oil temperature of an oil bath is increased to 120-140 DEG C, and the mixed solution is reacted for 2-4h, the generated methanol is separated out during the reaction, then the mixed solution is subjected to vacuum distillation for 2h, and the N-(ethoxycarbonylphenyl)-N'-methyl-N'-phenylformamidine product is obtained by filtration, in the application, the product has high selectivity and high conversion rate in the synthesis, and the zeolite catalyst can also adsorb the pigment of the product, so that the color value of the product is reduced.

The invention discloses a synthesis method of a derivative of a benzimidazole compound, which comprises the following steps: (1) uniformly mixing a reaction substrate, trimethyl orthoformate and acetic acid in the presence of a catalyst for reaction to obtain a benzimidazole intermediate product; and (2) dissolving the benzimidazole intermediate product obtained in the step (1), a halogenated compound and a coupling catalyst in a solvent, uniformly mixing and reacting to obtain a target product. The synthesis method disclosed by the invention is mild in reaction condition, and participation of an oxidizing agent and a reducing agent is avoided, so that a sensitive molecular structure is protected; the types of reaction substrates are wide, and are not limited to the range in which only aldehyde groups are used as the substrate; the reaction does not need a substrate with an aldehyde group, a corresponding product is obtained through coupling of 2-H benzimidazole and halogen, the situation that the substrate aldehyde is unstable or expensive and not easy to obtain is avoided, the practicability is higher, and the application range is wider.

The invention relates to a preparation method of methyl 3, 4-dihydroxy-5-methoxybenzoate, gallic acid is used as a raw material and reacts with trimethyl orthoformate or trimethyl orthoacetate, on one hand, the trimethyl orthoformate or trimethyl orthoacetate can protect o-diphenolic hydroxyl, on the other hand, the trimethyl orthoformate or trimethyl orthoacetate can also protect the o-diphenolic hydroxyl, and on the other hand, the trimethyl orthoformate or trimethyl orthoacetate can also protect the o-diphenolic hydroxyl; on the other hand, carboxyl esterification and 5-hydroxyl methylation can be performed to form 5-phenolic hydroxyl methylated and 3, 4-orthoester protected methyl benzoate as shown in a formula 1a or a formula 1b, and further acid solution treatment and deprotection are performed to prepare the target product 3, 4-dihydroxy-5-methoxy methyl benzoate. The preparation method is mild in reaction condition, simple in process, convenient to operate and high in product yield and purity, solves the problem of wastewater in a borax protection method, avoids using highly toxic dimethyl sulfate for methylation, is simple in process condition, convenient to operate and convenient to industrialize, and has extremely high application value.

The invention relates to a 3-methylene-2, 3-dihydro-4-quinolinone derivative and a synthetic method and application thereof.The synthetic method includes the steps that S1, an o-iodine / bromaniline derivative 2 and propargyl alcohol are subjected to a Sonogashira coupling reaction, and a 3-(2-aminophenyl) propane-2-alkyne-1-alcohol derivative 3 is obtained; s2, under the action of pyridine, the 3-(2-aminophenyl) propan-2-alkyne-1-alcohol derivative 3 and sulfonyl chloride are subjected to a reaction, and a sulfonyl protected 3-(2-aminophenyl) propan-2-alkyne-1-alcohol derivative 4 is obtained; and S3, carrying out Meyer-Schuster rearrangement reaction on three components, namely the 3-(2-aminophenyl) propane-2-alkyne-1-alcohol derivative 4 protected by sulfonyl, an aldehyde compound with R1 and trimethyl orthoformate, so as to obtain the 3-methylene-2, 3-dihydro-4-quinolinone derivative 1, namely, the 3-(2-aminophenyl) propane-2-alkyne-1-alcohol derivative 4 protected by sulfonyl, an aldehyde compound with R1 and trimethyl orthoformate. Compared with the prior art, the 3-methylene-2, 3-dihydro-4-quinolinone derivative disclosed by the invention is a neuraminidase inhibitor with a novel structure, can be applied to the anti-cancer, antibacterial and antiviral fields and the like, and is simple in synthetic route, simple in steps and convenient to operate.