19 results about "Cycloheptene" patented technology

The invention relates to the field of polyacrylate photoresists, in particular to a photoresist film-forming resin raw material and a preparation method thereof.The preparation method comprises the steps that cyclopentadiene is dropwise added into a mixed solution of alpha-bromomethyl acrylate and a solvent, the temperature is controlled, a reaction is conducted for 4 h, and 5-bromodicyclohept-2-ene-5-carboxylic acid methyl ester is prepared; the preparation method comprises the following steps: adding alkali into 5-bromo dicycloheptyl-2-ene-5-carboxylic acid methyl ester, and hydrolyzing at 20-30 DEG C for 2 hours to obtain a hydrolysis product; the hydrolysis product is subjected to epoxidation and hydrolysis with hydrogen peroxide under the condition of glacial acetic acid, and 1-bromine-5-hydroxy-3-oxa-tricyclic nonyl-2-ketone is obtained; according to the method, 1-bromo-5-hydroxy-3-oxa-tricyclic nonyl-2-ketone is cyanided by cuprous cyanide to prepare the 1-cyano-5-hydroxy-3-oxa-tricyclic nonyl-2-ketone monomer, and the method has the advantages that the raw materials are convenient and easy to obtain, the route is short, the reaction conditions are relatively mild, the operation safety is relatively high, the total yield is remarkably improved, and the like.

A cycloheptenone adduct of flavanols and stilbene compounds as shown in formula (I), its preparation method, and its use in treating cerebral ischemia. The compound of this invention has a simple preparation method and exhibits good neuroprotective activity.

The application relates to the field of organic synthesis and discloses a method for synthesizing campholenic aldehyde, which comprises the following steps: contacting 2,6,6-trimethyl-bicyclo[3.1.1]hept-2-ene and an oxidant in the presence of a first catalyst and a second catalyst, wherein the oxidant is an organic solution of a neutral organic peroxide, the first catalyst is an oxidation catalyst, and the second catalyst contains alkali metals and / or alkaline earth metals. The method can directly prepare campholenic aldehyde through two reactions of epoxidation and isomerization rearrangement in the same reaction system, the reaction process is reduced, the selectivity and yield of the campholenic aldehyde product are relatively high, the catalyst is easy to separate and has high recycling utilization rate, and the method has the advantages of simple operation steps and low production cost.

The invention discloses a pressure-sensitive adhesive for an anti-static polaroid protective film and a preparation method thereof, and the pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 30-40 parts of a water-based acrylate pressure-sensitive adhesive, 10-20 parts of Arabic gum, 10-20 parts of carrageenan, 2-acrylic acid-hexahydro-4, 4, 6-trimethyl-1, 3-pentanediol monoisobutyrate, 1-3 parts of a surfactant, 1-3 parts of an anti-static agent, 1-3 parts of an anti The preparation method comprises the following steps: adding 1 to 3 parts of 2, 7-methylene-1H-indenyl ester, 1 to 3 parts of 5-vinyl bicyclo [2.2. 1] heptyl-2-ene, 1 to 3 parts of a rosinyl acrylamide monomer, 5 to 8 parts of 1-allyl-3-vinyl imidazole chlorine salt, 0.8 to 1.5 parts of a hyperbranched water-soluble conjugated polymer, 0.5 to 1.5 parts of N-(4-cyano-3-trifluoromethylphenyl) methacrylamide, 0.3 to 0.6 part of vinylethylene carbonate and 1 to 3 parts of N-acryloylmorpholine into a reaction kettle; 0.5 to 1.5 parts of an initiator and 15 to 25 parts of water. The pressure-sensitive adhesive has the advantages of good bonding performance, excellent antistatic performance, high temperature and high humidity resistance, good aging resistance and high light transmittance.

The invention provides a preparation method of an enantiomer impurity of a key intermediate of meloabalin besylate, the chemical name of the enantiomer impurity of the key intermediate of meloabalin besylate is (1S, 5R)-3-ethyl-bicyclo [3.2. 0] heptane-3-ene-6-ketone, racemate 3-ethyl-bicyclo [3.2. 0] heptane-3-ene-6-ketone is used as a raw material, and the enantiomer impurity of the key intermediate of meloabalin besylate is prepared through a one-pot method. And adding reductase into the racemate to carry out reduction reaction, adding acid anhydride to react again after the reduction reaction, and carrying out alkali washing to obtain the enantiomer impurity of the meloabalin besylate key intermediate. According to the invention, a specific enzyme is found, the (1R, 5S)-3-ethyl-bicyclo [3.2. 0] heptane-3-ene-6-ketone can be specifically reduced, the treatment process is simple, the treatment capacity is large, expensive HPLC (High Performance Liquid Chromatography) chiral resolution is avoided, and the synthesis cost is greatly reduced.

The invention belongs to the field of molecular biology and enzyme engineering, and provides a transaminase mutant which can catalyze resolution of high-concentration 3-ethyl bicyclo [3.2. 0] hept-3-ene-6-ketone to obtain (1R, 5S)-3-ethyl bicyclo [3.2. 0] hept-3-ene-6-ketone (DB01). The method provided by the invention solves the problems of many ketol post-treatment steps, high cost, easy deterioration of a ketone substrate in the separation process and the like in the existing industrial synthesis route, and has a wide market prospect.

The invention relates to the technical field of synthesis of a 5H-dibenzo [a, d] cycloheptene skeleton, in particular to a synthesis method of the 5H-dibenzo [a, d] cycloheptene skeleton. Comprising the following steps: sequentially adding a catalyst, a ligand, alkali, a reactant I, a reactant II, a p-xylene solution and a magneton 5 into a reactor, connecting a condensing pipe, introducing condensed water from bottom to top, putting the reactor into an oil bath pan at 60-100 DEG C, heating, stirring and reacting for 6-24 hours, terminating the reaction, and purifying the product to obtain a 5H-dibenzo [a, d] cycloheptene skeleton product; the reactant I comprises 2-(2-bromophenyl)-1-acetophenone, 2-(2-bromophenyl)-1-(4-methylphenyl) ethanone, 2-(2-bromo-5-methylphenyl)-1-acetophenone or 2-(2-bromo-4-methoxyphenyl)-1-acetophenone, and the reactant II comprises 2-(2-bromophenyl)-1-(4-methylphenyl) ethanone, 2-(2-bromo-5-methylphenyl)-1-acetophenone or 2-(2-bromo-4-methoxyphenyl)-1-acetophenone; the reactant II comprises bicyclo [2.2. 1] heptyl-2, 5-diene-2, 3-dimethyl dicarboxylate, and the reactant II comprises bicyclo [2.2. 1] heptyl-2, 5-diene-2, 3-dimethyl dicarboxylate; the method is mild in reaction condition, high in selectivity, relatively high in yield and environment-friendly; the active product can be used in the field of synthesis of drugs, pesticides and paint dyes.

The invention provides fluorinated derivatives of methoxydibenzo[b,f]oxepin of general formula (1) and general formula (2) and a method for obtaining thereof in a catalysed reaction of fluoroazobenzene with methoxydibenzo[b,f]oxepin. The preferable catalyst of the reaction is triethylamine, and the compounds obtained may be useful as molecular switches in biological systems and photopharmacology.

The application provides a kind of oxo-bridged bicyclo-[2.2.1]-heptene compounds containing different sulfonamide nitrogen atom substituent groups and its preparation method and application, in the application, dienophile compound containing different sulfonamide nitrogen atom substituent groups and 3,4-diphenol furan / 3,4-diphenol furan containing halogen substitution are used as raw materials, oxo-bridged bicyclo-[2.2.1]-heptene compounds containing different sulfonamide nitrogen atom substituent groups are prepared by solvent-free reaction at 90 DEG C in one step;Such compounds show certain inhibitory activity and protein degradation activity on wild-type breast cancer cells MCF-7 and three drug-resistant mutant breast cancer cells MCF-7Y537S, MCF-7D538G, MCF-7EGFR;And oxo-bridged bicyclo-[2.2.1]-heptene compounds containing fluorine atom or chlorine atom substitution on benzene ring improve the affinity for estrogen receptor, and interfere with estrogen receptor dimerization interface, which is a new mechanism of estrogen receptor inhibitor for anti-breast cancer drug-resistant mutation.

Disclosed are dimethylbicycloheptenyl and dimethylbicycloheptanyl derivatives possessing green-galbanum and fruity-pineapple odor notes.

Functionalized benzocycloheptenes are one of the most important classes of bicyclic framework that have been investi-gated in different areas of biological activities. The claimed invention provides preparations of benzocycloheptene analogues, inhibitors of PI3K and MK2, pharmaceutical compositions containing them and their use in therapy. The compounds of Formula I, II, III, IV, V and VI may be used as anti type 2 diabetes, antipyretic, anti-inflammatory, antiepileptic, anticancer, antiulcer, CNS-stimulant, and CNS-depressant. These benzocycloheptene derivatives are useful in treatment of PI3K and MK2 related disorders.

The invention belongs to the technical field of medicinal chemistry, and particularly relates to a photocatalytic preparation method of a milobalin intermediate. Comprising the following steps: dissolving (1S, 5R)-3-ethyl-bicyclo [3.2. 0] hept-3-en-6-one in a solvent, adding a photosensitizer, carrying out a reaction under light with a specific wavelength and at a temperature, and after the reaction is finished, carrying out post-treatment to obtain the 3-ethyl-bicyclo [3.2. 0] hept-3-en-6-one racemate, namely (1S, 5R)-3-ethyl-bicyclo [3.2. 0] hept-3-en-6-one racemate, namely (1S, 5R)-3-ethyl-bicyclo [3.2. 0] hept-3-en-6-one racemate and (1S, 5R)-3-ethyl-bicyclo [3.2. 0] hept-3-en-6-one racemate. The yield is good and the purity is high. And the recycling of the waste compound (1S, 5R)-3-ethyl bicyclo [3.2. 0] hept-3-ene-6-ketone is realized.

The application discloses a kind of 3-alkyl bicyclo [3.2.0] hept-3-en-6-ketone resolution method, belong to the field of medicinal chemistry. Including the following steps: (1) the racemic mixture of 3-alkyl bicyclo [3.2.0] hept-3-en-6-ketone and aprotic polar solvent are added to reaction bottle, and the mixture is obtained;(2) under stirring, (1) mixture is added to the resolution reagent in step, and the reaction product is obtained after reaction, and the optical purity ee. After post-treatment of reaction product, (1R,5S) -3-alkyl bicyclo [3.2.0] hept-3-en-6-ketone with 98% is obtained. The method of the application is simple in operation steps, low in material cost, and high in optical purity of product.

The present invention discloses a process for the synthesis of a compound according to formula (I) or a pharmaceutically acceptable salt thereof, wherein - R is a bicycloalkyl group, preferably an unsubstituted bicycloalkyl group. The process the following steps, preferably performed sequential in time, I. asymmetric ring opening of a carbic anhydride, preferably cis-5-Norbornene-endo-2,3-dicarboxylic anhydride or (3aR,4S,7R,7aS)-3a,4,7,7a-tetrahydro-4,7- methanoisobenzofuran-1,3-dione, yielding (1S,2R,3S,4R)-3- (methoxycarbonyl)bicyclo[2.2.1]hept-5-ene-2-carboxylic acid, II. epimerizing of (1S,2R,3S,4R)-3-(methoxycarbonyl)bicyclo[2.2.1]hept-5-ene-2- carboxylic acid yielding (1S,2R,3R,4R)-3-(methoxycarbonyl)bicyclo[2.2.1]hept-5-ene- 2-carboxylic acid, III. hydrogenating (1S,2R,3R,4R)-3-(methoxycarbonyl)bicyclo[2.2.1]hept-5-ene-2- carboxylic acid yielding (1R,2R,3R,4S)-3-(methoxycarbonyl)bicyclo[2.2.1]heptane-2- carboxylic acid, IV. decarboxylating (1R,2R,3R,4S)-3-(methoxycarbonyl)bicyclo[2.2.1]heptane-2- carboxylic acid yielding methyl (1S,2S,4R)-bicyclo[2.2.1]heptane-2-carboxylate, V. hydrolysing methyl (1S,2S,4R)-bicyclo[2.2.1]heptane-2-carboxylate yielding (1S,2S,4R)-bicyclo[2.2.1]heptane-2-carboxylic acid, VI. coupling (1S,2S,4R)-bicyclo[2.2.1]heptane-2-carboxylic acid with a benzylamine, preferably substituted with a substituent selected from the group consisting of heteroatoms, in particular F, SF5, CF3 or OCF3, or an alkyl group, in particular an ethyl-, methyl- or propyl-group, yielding a compound according to formula (I), and VII. optionally crystallising of the compound according to formula (I).

The application belongs to the field of plant protection, and particularly relates to a kind of western flower thrips luring composition and application. The western flower thrips luring composition is composed of 1,3-dimethylbenzene, p-xylene, 1,7,7-trimethyltricycloheptane, 1R-alpha-pinene and 2,6,6-trimethyl-bicyclohept-2-ene. The above-mentioned five kinds of compounds are obtained by enriching zucchini volatiles, separating and screening volatiles, and are mixed to prepare the western flower thrips luring composition according to the volume ratio. The field test results of the western flower thrips luring composition show that the western flower thrips luring composition has significant luring activity on western flower thrips, is simple to prepare, is friendly to the environment, is non-toxic to human and livestock, and has good popularization and application prospect.

The invention provides a stable pharmaceutical composition containing [(1R, 5S, 6S)-6-(aminomethyl)-3-ethyl bicyclo [3.2. 0] hept-3-ene-6-yl] acetic acid or single benzene sulfonate thereof, and the pharmaceutical composition contains an effective amount of active substances and a stabilizer, and has excellent industrial application value.

The present application relates to bicyclic heptenyl amino substituted azaheterocyclic compounds and their medical uses, the structure is shown as formula (I). The present application also relates to the preparation method of the compounds, pharmaceutical compositions and their use as FGFR4 inhibitors in the treatment of cancer.

The purpose of the present disclosure is to provide a compound that is useful in a production method, said compound making it possible to solve at least one issue selected from 1) making HCN management unnecessary, 2) making heavy metals such as Co and Ni unnecessary, and 3) making a pressurized container unnecessary, when producing mirogabalin. The present disclosure relates to a bicycloheptene compound represented by formula (I). (In formula (I), X represents -CN or -C(=O)NH2. Y represents a hydrogen atom or -CO2T. T represents a hydrogen atom or a C1-3 alkyl group.)

The invention provides a method for separating and detecting impurities in a melogabalin intermediate and a reagent composition. According to the separation method, 2-((1R, 5S, 6S)-6-(aminomethyl)-3-ethyl bicyclo [3.2. 0] hept-3-ene-6-yl) tert-butyl acetate mandelate and diastereoisomer impurities thereof are separated by adopting chromatography, a mobile phase of the chromatography comprises a salt solution, acetonitrile and tetrahydrofuran, and the pH value of the salt solution is greater than 7 and less than 10. According to the method, the melogabalin intermediate and the diastereoisomer thereof can be effectively separated, and the content of the diastereoisomer can be accurately measured.