Patent classifications
C07C235/82
Method for preparing 1,3-dicarbonyl compound based on metal hydride/palladium compound system
Disclosed is a method for preparing a 1,3-dicarbonyl compound based on a metal hydride/palladium compound system. The method includes the following steps: suspending a palladium compound and a metal hydride in a solvent under the protection of nitrogen, then adding an electron-deficient olefin compound, reacting same at 0° C.-100° C. for 0.3 to 10 hours, then adding a saturated ammonium chloride aqueous solution to stop the reaction, and then subjecting same to extraction, evaporation until dryness, and column chromatography purification to obtain the 1,3-dicarbonyl compound. The hydride and palladium compound catalysts used by the present invention are reagents easily obtained in a laboratory. Compared to a common hydrogen hydrogenation method, the method is easier to operate, and has a higher safety, mild conditions, and a high reaction yield.
Method for preparing 1,3-dicarbonyl compound based on metal hydride/palladium compound system
Disclosed is a method for preparing a 1,3-dicarbonyl compound based on a metal hydride/palladium compound system. The method includes the following steps: suspending a palladium compound and a metal hydride in a solvent under the protection of nitrogen, then adding an electron-deficient olefin compound, reacting same at 0° C.-100° C. for 0.3 to 10 hours, then adding a saturated ammonium chloride aqueous solution to stop the reaction, and then subjecting same to extraction, evaporation until dryness, and column chromatography purification to obtain the 1,3-dicarbonyl compound. The hydride and palladium compound catalysts used by the present invention are reagents easily obtained in a laboratory. Compared to a common hydrogen hydrogenation method, the method is easier to operate, and has a higher safety, mild conditions, and a high reaction yield.
A PROCESS METHOD FOR PRODUCING PESTICIDE BY USING CARBON DIOXIDE
A process method for producing pesticide by using carbon dioxide comprises the following steps: Weighing 1, 3-cyclohexanedione substrate, catalyst and Cs2CO3 in Schleck bottle, degassing, and continuously introducing 1 atm of carbon dioxide. Add solvent and react for 48 h in an oil bath at 50° C. After the reaction was completed, post-treatment was carried out to obtain 2(a-e). The obtained acid is acylated and then added dropwise to dichloromethane solution containing aniline to react for 2 h at normal temperature. After the reaction, column chromatography was performed to obtain 3(a-e). Add 3 (a-e) into 50% concentrated sulfuric acid and reflux at 80° C. for 8 hours. Through separation, 4(a-e) was obtained. The invention has the advantages that the catalyst is simple to prepare, has high catalytic activity, can be recycled, realizes industrial circulation, and achieves the goal of sustainable production. The preparation process of 3(a-e) and 4 (a-e) is simple, with low requirements on equipment, wide sources of raw materials, low cost, low toxicity and easy industrial scale-up production.
A PROCESS METHOD FOR PRODUCING PESTICIDE BY USING CARBON DIOXIDE
A process method for producing pesticide by using carbon dioxide comprises the following steps: Weighing 1, 3-cyclohexanedione substrate, catalyst and Cs2CO3 in Schleck bottle, degassing, and continuously introducing 1 atm of carbon dioxide. Add solvent and react for 48 h in an oil bath at 50° C. After the reaction was completed, post-treatment was carried out to obtain 2(a-e). The obtained acid is acylated and then added dropwise to dichloromethane solution containing aniline to react for 2 h at normal temperature. After the reaction, column chromatography was performed to obtain 3(a-e). Add 3 (a-e) into 50% concentrated sulfuric acid and reflux at 80° C. for 8 hours. Through separation, 4(a-e) was obtained. The invention has the advantages that the catalyst is simple to prepare, has high catalytic activity, can be recycled, realizes industrial circulation, and achieves the goal of sustainable production. The preparation process of 3(a-e) and 4 (a-e) is simple, with low requirements on equipment, wide sources of raw materials, low cost, low toxicity and easy industrial scale-up production.
CARBON-MONOXIDE-RELEASING MOLECULES AND THERAPEUTIC APPLICATIONS THEREOF
Carbon monoxide-releasing organic molecules are described herein. The molecules can be synthesized prior to administration (e.g., ex vivo) or formed in vivo. In those embodiments where the molecules are formed in vivo, reactants are administered under physiological conditions and undergo a cycloaddition reaction to form a product which releases carbon monoxide. In applying such reactions for therapeutic applications in vivo, the cycloaddition and CO release typically occur only under near-physiological or physiological conditions. For example, in some embodiments, the cycloaddition reaction and/or release of carbon monoxide occur at a temperature of about 37° C. and pH of about 7.4. Pharmaceutical compositions and methods for release carbon monoxide are also described.
COMBINATORIAL ANTIBIOTIC DERIVATIVES BASED ON SUPRAMOLECULAR STRUCTURES
Field of application: The invention relates to combinatorial chemistry, pharmacy and cosmetology, allows to synthesize new combinatorial libraries of derivatives of antibiotics for use in pharmacy, cosmetology and pharmacy.
Technical result: modified combinatorial derivatives of antibiotics with antimicrobial and antifungal activity against multiresistant and pan drug resistance strains of microorganisms and fungi. Means have a wide spectrum of action, and the supramolecular and combinatorial structure of their tens and hundreds of derivatives eliminates the resistance of microorganisms.
COMBINATORIAL ANTIBIOTIC DERIVATIVES BASED ON SUPRAMOLECULAR STRUCTURES
Field of application: The invention relates to combinatorial chemistry, pharmacy and cosmetology, allows to synthesize new combinatorial libraries of derivatives of antibiotics for use in pharmacy, cosmetology and pharmacy.
Technical result: modified combinatorial derivatives of antibiotics with antimicrobial and antifungal activity against multiresistant and pan drug resistance strains of microorganisms and fungi. Means have a wide spectrum of action, and the supramolecular and combinatorial structure of their tens and hundreds of derivatives eliminates the resistance of microorganisms.
AN IMPROVED PROCESS FOR THE PREPARATION OF CABOZANTINIB AND ITS PHARMACEUTICALLY ACCEPTABLE SALTS THEREOF
The present invention relates to an improved process for the preparation of N-(4-(6,7-dimethoxyquinolin-4-yloxy)phenyl)-N′-(4-fluorophenyl)cyclopropane-1,1-dicarboxamide compound of formula-1 which is represented by the following structural formula:
##STR00001##
AN IMPROVED PROCESS FOR THE PREPARATION OF CABOZANTINIB AND ITS PHARMACEUTICALLY ACCEPTABLE SALTS THEREOF
The present invention relates to an improved process for the preparation of N-(4-(6,7-dimethoxyquinolin-4-yloxy)phenyl)-N′-(4-fluorophenyl)cyclopropane-1,1-dicarboxamide compound of formula-1 which is represented by the following structural formula:
##STR00001##
APPLICATION OF METAL HYDRIDE/PALLADIUM COMPOUND SYSTEM IN PREPARATION OF 1,3-DICARBONYL COMPOUND IN CASCADE REACTION OF ELECTRON-DEFICIENT ALKENE COMPOUND
Provided is an application of a metal hydride/palladium compound system in the preparation of a 1,3-dicarbonyl compound in a cascade reaction of an electron-deficient alkene compound, said reaction comprising the following steps: under the protection of nitrogen, a palladium compound and a metal hydride are suspended and stirred in a solvent, then an electron-deficient alkene compound is added; the mixture reacts at 0 C. to 100 C. for 0.3 to 10 hours; a saturated ammonium chloride aqueous solution is added to stop the reaction, and then extraction, drying by evaporation and purification by column chromatography are performed to obtain the product of 1,3-dicarbonyl compound. The hydride and palladium compound catalysts used in the method are reagents easily obtained in a laboratory; compared with the commonly used methods of hydrogenation with hydrogen gas, the method can be easily operated, and has high safety, mild conditions and high reaction yield.