44results about How to "Process selection is reasonable" patented technology

The invention explores a method for synthesizing and refining cinacalcet hydrochlorid, especially avoids toxic and expensive reaction reagents reported in literatures; the invention has the advantages of convenient sources of raw materials and reagents, low cost, little pollution to environment and simple operation, the invention is suitable for industrial production.

The invention relates to a novel method for synthesizing 5-trifluoromethyl-1-indanone. The method comprises the following steps: adopting industrial m-trifluoromethyl benzaldehyde as raw material and preparing m-trifluoromethyl cinnamic acid by Knoevenagel condensation; hydrogenating to obtain m-trifluoromethyl phenylpropionic acid; and preparing 5-trifluoromethyl-1-indanone by intramolecular Friedel-Crafts acylation. The first step is carried out in the presence of malonic acid as organic reagent and pyridine or piperidine as catalyst under reflux at 100 DEG C. The second step is carried out in the presence of palladium/carbon or palladium hydroxide/carbon as catalyst and reaction solvent such as methanol, ethanol, ethyl acetate or tetrahydrofuran under a pressure of 40psi at room temperature. The third step is carried out with trifluoromethanesulfonic acid for closing rings at -20 DEG C-90 DEG C. The method provides a synthesis process for 5-trifluoromethyl-1-indanone which is simple and easy to be scaled, and solves the technical problems in prior art on relative long synthetic route, expensive catalyst or raw material, and severe reaction conditions, high cost, etc.

The invention discloses a preparation method of 1,4-diallyl isoquinoline synthesized by using a palladium catalyst. The structural formula of 1,4-diallyl isoquinoline is shown in the specification, wherein R1 refers to one or more substituents connected to a benzene ring, and is selected from one of H, chlorine and -O-CH2-O-, and R2 is one of phenyl, p-methoxyphenyl, and 1-cyclohexenyl. In the process of preparing, 1-methyl azide-2-ethinyl-benzene shown in the specification is taken as a raw material, and reacted with allyl methyl carbonate in the presence of a Pd(PPh3)4 catalyst, an alkaline cocatalyst and an organic solvent, so that 1,4-diallyl isoquinoline is obtained. According to the invention, a 1,4-diallyl isoquinoline compound can be efficiently synthesized by using a one-pot method; the preparation method is high in conversion efficiency, short in reaction time and neutral in reaction conditions, and has no generated by-product; the method is low in raw material cost, simple in operation, low in pollution to the environment, and beneficial to industrialized production; and products are widely used, and can be used as intermediates for further synthesizing more complex compounds.

This invention relates to a method for preparing 2-amino-8-nonenoic acid, especially optically active 2-amino-8-nonenoic acid. The method overcomes the problems of long synthesis route, low yield and expensive chiral catalyst or resolution reagent faced by the present method. The method comprises: attacking chiral pyroglutamate containing protecting groups with Grignard reagent of crotyl bromide to obtain chiral 2-amino-5-oxy-8- nonanoate, reducing to remove carbonyl and obtain chiral or racemized 2-amino-8-nonanoate, and hydrolyzing to obtain optically active 2-amino-8-nonenoic acid. The method in this invention has such advantages as simple route, reasonable process, and high yield, and is suitable for mass production.

The invention discloses a synthetic method of 8-isoquinolinol, and belongs to the field of synthesis method of isoquinoline compounds. The synthetic method comprises following steps: 8-chloroisoquinoline, copper acetylacetonate, lithium hydroxide monohydrate, and ligand 1,3-bis(4-hydroxyl-2,6-dimethyl phenyl)urea are added into a mixed solution of dimethyl sulfoxide and water; under nitrogen protection, an obtained reaction solution is subjected to heating with stirring until reaction is completed, and pH value is adjusted to 5 with HCl after cooling; an obtained mixed liquid is extracted with ethyl acetate, an obtained organic phase is washed with saturated salt solution, is dried with anhydrous sodium sulfate, and then is subjected to spin drying; and an obtained crude product is subjected to column chromatography separation so as to obtain 8-isoquinolinol. According to the synthetic method, 8-chloroisoquinoline is taken as a raw material; synthesis route is simple; the synthetic method is reasonable; the raw materials are easily available; operation and subsequent treatment are convenient; total yield is as high as 72%; amplify production is convenient to realize; and large-scale production of 8-isoquinolinol can be realized.

The invention relates to a method for synthesizing 1-R-2, 3-dihydrogen-1H-quinoline-4-ketone, which mainly solves the technical problems that the prior synthesis method is difficult to amplify raw material, long in route, inconvenient in reaction operation, and the like. The method for synthesizing 1-R-2, 3-dihydrogen-1H-quinoline-4-ketone is characterized by comprising the following steps: a. 4-hydroxyquinoline is taken as a raw material and reacts with alkyl halogenated matter, benzyl halogenated matter or alkyl sulphonic acid ester in solvent to form ketene; b. the ketene dissolves in the solvent, and a reducing agent is added to the solvent so as to obtain corresponding alcohol; and c. oxidant is added to the corresponding alcohol dissolved in the solvent, so as to obtain the 1-R-2, 3-dihydrogen-1H-quinoline-4-ketone through oxidation.

The invention provides a 5-bromo-7-trifluoromethyl quinoline synthetic method. The 5-bromo-7-trifluoromethyl quinoline synthetic method comprises the following steps of by taking m-trifluoromethylaniline as a starting material, performing Skraup condensation to obtain 7-trifluoromethyl quinoline, and then performing reaction on the 7-trifluoromethyl quinoline and NBS to obtain 5-bromo-7-trifluoromethyl quinoline. According to the 5-bromo-7-trifluoromethyl quinoline synthetic method provided by the invention, a synthetic route of the method eliminates the disadvantages of incapability of purification, low yield and the like of a product in the existing synthetic technology, and the 5-bromo-7-trifluoromethyl quinoline synthetic method has the advantages of concision in synthetic route, reasonability in technology selection, low cost in raw materials, simpleness and availability in raw materials, convenience in operation and aftertreatment, high total yield and the like.

The invention provides a synthetic method of 3-bromo-7-methoxyl quinoline. The synthetic method of 3-bromo-7-methoxyl quinoline comprises the following steps: 1) adding a solvent into 7-nitryl-1,2,3,4-tetrahydroquinoline, adding DDQ and stirring the mixture to react to obtain 7-nitryl quinoline, wherein the molar ratio of 7-nitryl-1,2,3,4-tetrahydroquinoline and DDQ is 1: (1-5); 2) adding the solvent into 7-nitryl quinoline, heating the mixture, adding N-bromo-succinimide to react to obtain 3-bromo-7-nitryl quinoline in an insulating manner; and 3) dissolving 3-bromo-7-nitryl quinoline in thesolvent, adding sodium methylate, and heating the mixture to stir and react to obtain 3-bromo-7-methoxyl quinoline. The synthetic method of 3-bromo-7-methoxyl quinoline is concise in synthetic route,reasonable in process selection, low in raw material cost, simple and easy, convenient to operate and post-treat, high in total yield and easy to amplify.

The invention discloses a synthesis method of 6- (trifluoromethyl) isoquinoline-5-ol, which comprises the following steps of by using p-trifluoromethyl phenylethylamine as a raw material, carrying outamino protection, cyclization, hydrolysis, bromination, debromination alkene insertion and dehydroaromatization on the p-trifluoromethyl phenylethylamine and TFAA to obtain 7-trifluoromethyl isoquinoline, and carrying out 5-site bromination on the 7-trifluoromethyl isoquinoline and NBS to generate 5-bromine- 7-trifluoromethyl isoquinoline, and carrying out methoxylation and demethylation with sodium methoxide to obtain 6-(trifluoromethyl) isoquinoline-5-alcohol. The method is simple in synthetic route, reasonable in process selection, low in raw material cost, simple and easily available in raw materials, convenient to operate and post-treat, high in total yield, free of highly toxic reagents and easy to amplify, and can be used for large-scale production.

The invention discloses a synthesis method of 3-aminopyridine formaldehyde, which comprises the following steps of: carrying out a cutius rearrangement reaction on 2-bromonicotinic acid serving as a raw material to obtain tert-butyl (2-bromopyridine-3-yl) carbamate, carrying out a Grignard reaction to obtain tert-butyl (2-formyl pyridine-3-yl) carbamate, and finally carrying out a hydrolysis reaction to obtain 3-aminopyridine formaldehyde. The synthesis method overcomes the defects of expensive raw materials, low yield, use of microwave reaction and other conditions, difficulty in amplification and the like in the existing synthesis process, and has the advantages of simple synthesis route, reasonable process selection, low raw material cost, simple and easily available raw materials, convenience in operation and post-treatment, high total yield, no use of highly toxic reagents, easiness in amplification, and realization of mass production.