39 results about "1-adamantanol" patented technology

The invention relates to a preparation method for Vildagliptin. The preparation method comprises the following steps: using L-prolinamide as a raw material, performing the dehydration reaction with cyanuric chloride, and generating (S)-2-cyanopyrrolidine; performing the salt forming reaction to the (S)-2-cyanopyrrolidine and hydrogen chloride, to obtain intermediate-1; enabling the intermediate-1 to react with chloroacetic acid under the conditions of using EDCI as a condensing agent, using HOBt as a catalyst, and using DIEA as an acid-binding agent, to obtain intermediate-2; enabling the intermediate-2 to react with 3-amino-1-adamantanol, to obtain the Vildagliptin, filtering, concentrating, crystallizing, and re-filtering to obtain a Vildagliptin crude product; and preparing the Vildagliptin finished product by the acetone refining. The preparation method is capable of providing a new method, and reducing the generation of by-products in each step. The content of the disubstitution product of the Vildagliptin by-product and the 3-amino-1-adamantanol are reduced to less than 0.1%, the yield and purity of the Vildagliptin are effectively improved, the raw materials are easily obtained, the conditions are moderate, and the preparation method is suitable for the industrial large-scale production.

The invention relates to a method for producing a 1-adamantanol product which is prepared by subjecting adamantane to bromination reaction and hydrolysis reaction. Bromine is used as a halogenating agent, and the dosage is one to ten times of the adamantane in mole number. A is used as a bromination catalyst, and the dosage is 0.5 percent to 5 percent of the weight of the adamantane. The temperature of the bromination reaction is 0 DEG C to 100 DEG C, and the reaction pressure is normal pressure. The invention is characterized in that the hydrolysis temperature of 1-bromine adamantane is 100 DEG C to 150 DEG C, and the reaction pressure is 0-3atm. The purity of the 1-adamantanol obtained by the invention is more than or equal to 99.5 percent, and the yield is more than 95 percent.

The invention discloses a novel preparation method of Vildagliptin. The preparation method comprises that L-prolinamide as a raw material, chloroacetyl chloride and tetrahydrofuran undergo an acylation reaction, the reaction product is subjected to suction filtration, the filtrate and trifluoroacetic anhydride directly undergo a dehydration reaction without filtrate separation purification to produce (-)-(2S)-1-chloroacetylpyrrolidine-2-carbonitrile (II), the refined (-)-(2S)-1-chloroacetylpyrrolidine-2-carbonitrile, 3-amino-1-adamantanol (III), potassium carbonate and potassium iodide undergo a reaction to produce (-)-(2S)-1-[[(3-hydroxytricyclo[3.3.1.1[3,7]]dec-1-yl)amino]acetyl]pyrrolidine-2-carbonitrile (I) in acetone, and the (-)-(2S)-1-[[(3-hydroxytricyclo[3.3.1.1[3,7]]dec-1-yl)amino]acetyl]pyrrolidine-2-carbonitrile (I) is refined by calcium double salt, ethyl acetate and butanone to form pure Vildagliptin (compound wg-0). The improved synthesis technology has the advantages of less reaction steps, operation simpleness, after-treatment simpleness, low employee cost, equipment cost and time cost, high yield, high product quality and industrialization feasibility.

The invention relates to a method and a device for continuous preparation of Vildagliptin by tubular reaction; 3-amino-1-adamantanol and 1-chloracetyl-2-cyano pyrrolidine are dissolved in a mixed solution of solvents, then dissolved with an alkali and a catalyst in a suspension of the solvents, mixed, and preheated by a preheater, the preheated mixed solution enters into a tubular reactor at 20-100 DEG C, the residence time of a material in the tubular reactor is 30min-180min, and the reaction solution discharged from the tubular reactor is collected, filtered washed and purified to obtain the product. The method greatly improves the response speed, shortens the production cycle, increases the amount of processing, and can effectively improve the production capacity. In addition, by controlling the reaction temperature, material movement speed, dosage ratio, catalyst amount and alkali dosage, the formation of by-products disubstituted compounds can be effectively avoided.

The invention discloses a method for synthesizing 3-amino-1-adamantanol. The structural formula of the 3-amino-1-adamantanol is as follows. Using adamantanecarboxylic acid as starting material, the method synthesizes the 3-amino-1-adamantanol according to the following reaction steps: bromate 3-amino-1-adamantanol is synthesized by way of bromination, modified curtius rearrangement and hydrolyzation, and finally, bromate is removed by a alkaline liquor treatment method, so that the 3-amino-1-adamantanol is obtained. The invention has the advantages of simple and easy operation, available materials, less reaction steps and high product yield.

The invention relates to a preparing method for vildagliptin and belongs to the field of compound preparation. The method comprises the following steps that under an amide organic solvent system and the existence of alkali, 3-amino-1-adamantanol and (S)-1-(2-chloroacetyl)pyrrolidine-2-carbonitrile are subjected to an alkylation reaction, and a reaction solution is obtained; then, the reaction solution is subjected to posttreatment, and vildagliptin is obtained. The method has the advantages that reaction raw materials and a solvent are saved, the yield is high, purity is high, the content of dipolymer impurities is low, the medicinal requirement is met, operation is simple, the reaction time is short, posttreatment is easy, and industrialization is promoted.

The invention discloses a process for preparing a vildagliptin intermediate 3-amino-1-adamantanol. According to the process, amantadine hydrochloride is taken as a starting raw material, and the 3-amino-1-adamantanol is obtained by carrying out a mixed acid reaction on H2SO4/HNO3, carrying out alkaline hydrolysis on KOH/H2O, and carrying out ethanol extraction. The process is characterized in thatseparation and purification can be performed by using an ethanol extraction process after the alkaline hydrolysis is finished, so that the product yield is greatly increased. The preparation processis easy in obtaining of raw materials, rapid in reaction and high in yield, thus being suitable for industrial production.

A process for synthesizing 3,5-disubstituent-1-adamantanol includes reaction between 1,3-disubstituent adamantane and bromine to obtain bromo compound, adding sodium oxalate and water, reaction, filtering and washing.

The present invention is a process for producing 2-adamantanol and 2-adamantanone from 1-adamantanol, by using as a catalyst a substance comprising at least one kind of acid catalyst selected from Lewis acid(s) and solid acid(s) that coexist with at least one kind selected from the group consisting of carboxylic acids, sulfonic acids, and phosphoric acids, and provides a process suitable for mass production of 2-adamantanol and 2-adamantanone selectively with high efficiency without using sulfuric acid as a catalyst, thereby enabling laborsaving in waste acid treatment step and drastic reduction of the reaction time.

The invention belongs to the field of chemical production, and in particular relates to a recovery and improvement device for producing 3-amino-1-adamantanol, comprising a reaction kettle, a centrifugal device and an extraction kettle; the centrifugal device includes a centrifuge barrel for centrifuging slurry; The upper end of the centrifuge bucket is provided with a centrifugal feed inlet for slurry and water to enter, and a centrifugal outlet for throwing out the discharge liquid when the slurry is centrifuged; the lower end is provided with a discharge outlet for the material generated after the slurry is centrifuged Centrifugal discharge port; the extraction kettle includes a kettle body, the inside of the kettle body is provided with a stirring mechanism, the top of the kettle body is provided with a sealing cover, and an extraction liquid feeding port, an extraction agent feed port, vent valve and extraction discharge port; the centrifugal feed port is connected with the bottom opening of the reaction kettle, and the centrifugal discharge port is connected with the extraction liquid feed port of the extraction kettle ; The extraction outlet is connected with the reaction kettle.

The invention discloses an improvement method for a synthesis process of memantine hydrochloride; with 1,3-dimethyl adamantane as a raw material, 3,5-dimethyl-1-adamantanol is obtained through a bromination reaction and a hydrolysis reaction; 3,5-dimethyl-1-adamantanol is subjected to a chlorination reaction to obtain 1-chloro-3,5-dimethyl adamantane; and 1-chloro-3,5-dimethyl adamantane is subjected to an ammoniation reaction, acid hydrolysis and salt formation, and the target product of methamine hydrochloride is produced, wherein in the bromination reaction, the reaction molar ratio of 1,3-dimethyl adamantane and bromine is 1:1.1, the reaction is performed in dichloroethane, and after the hydrolysis reaction, an organic phase is separated and washed to remove bromine and washed and dried, and an obtained solution is directly used for a next reaction. The improvement method provided by the invention can improve the yield, increase reaction safety and reduce waste and waste water.

The invention belongs to the field of chemical production, and particularly relates to a 3-amino-1-adamantanol production improvement device. The 3-amino-1-adamantanol production improvement device comprises a reaction liquid storage tank, a magnetic drive pump, and a reaction kettle provided with a stirring paddle, wherein the reaction liquid storage tank, the magnetic drive pump and the reaction kettle are sequentially connected through a liquid delivery tube; an ultrasound device is arranged between the reaction liquid storage tank and the magnetic drive pump and comprises a box body, an ultrasound concussion board arranged in the box body, and an ultrasound generation device arranged outside the box body and connected with the ultrasound concussion board; an inlet end of the box body is connected with the bottom part of the reaction liquid storage tank, and an outlet end of the box body is connected with the magnetic drive pump. The bottom part of the reaction kettle is connected with an inlet of the reaction liquid storage tank. The ultrasound concussion board of the ultrasound device shocks and breaks bubbles so as to greatly reduce the phenomenon of gas-including liquid, the content of the individual impurity of a finished product of 3-amino-1-adamantanol is reduced to be lower than 0.3%, and the content of the product is improved.

The invention discloses a trans-4-aminoadamantan-1-ol hydrochloride synthesis technology. The technology comprises that 4-amino-1-adamantanol is prepared from 5-hydroxy-2-adamantanone as a raw material through hydroxylamine hydrochloride oximation and Raney nickel hydrogenation reduction, the 4-amino-1-adamantanol is acidized to form a salt and trans-4-aminoadamantan-1-ol hydrochloride is prepared from the salt through methanol recrystallization three-step reactions. Compared with the prior art reported through the existing patent literature, the technology has the advantages of simple processes, raw material easy acquisition, low cost and high yield.

The invention discloses jack oil used at an ultralow temperature. The jack oil is prepared from the following components in parts by weight: 99 parts of hydrogenated tail oil, 0.1-0.3 part of an antirust agent, 0.2-0.4 part of an antioxidant, and 0.5-0.7 part of a functional agent, wherein the functional agent is prepared from the following components in parts by weight: 60-70 parts of 1-adamantanol, 10-12 parts of 3-nonanol, and 6-8 parts of tetra-n-butyl titanate. The jack hydraulic oil prepared by the method provided by the invention can work normally in an ultralow-temperature environment, and greatly improves the performance and the application range of a jack.