120results about How to "The post-processing method is simple" patented technology

The invention relates to a new preparation route and a new method for a p-toluenesulfonic acid edoxaban hydrate and intermediates thereof. The new method comprises the steps that a high-reactivity compound 109A4x is prepared; a compound 109C6x is prepared by using a new synthesizing method; new compounds 109E8-01, 109E9x and 109T7-01 are prepared; the p-toluenesulfonic acid edoxaban hydrate is prepared by using the intermediates. By using the new method and the new route, the reaction step of copious cooling is omitted, and dangerous elemental sulfur, high-risk n-butyllithium and high-risk azides are prevented from being used. In a word, by means of the method, the p-toluenesulfonic acid edoxaban hydrate and the key intermediates thereof are more easily and safely prepared at a lower coston an industrialization scale.

The invention relates to a preparation method of L-alanyl-L-glutamine; the preparation method comprises the following steps of: a) adding a solvent to a reaction container; stirring the solvent; and then adding N-phthaloyl-L-alanyl-L-glutamine to the reaction container; putting the reaction container in an ice bath; dripping a short-chain amine solution into a solution for clarification; removing the ice bath; adding the rest short-chain amine solution to the solution; after finishing dripping, carrying out room temperature reaction on the solution; decompressing and concentrating the solution to remove excessive short-chain amine in a water bath until the pH value of the solution is 6-7; standing for crystallization; filtering crystals; and drying filter cakes at a normal pressure so as to obtain a crude product; and b) adding water to the crude product at room temperature; dissolving the crude product in the water; dripping short-chain alcohol into the water for crystallization and purification during stirring, so as to obtain the L-alanyl-L-glutamine. Through the adoption of the preparation method of the L-alanyl-L-glutamine provided by the invention, hypertoxic hydrazine hydrate is avoided; and the preparation method of the L-alanyl-L-glutamine provided by the invention has the advantages of greater safety in operation, high product purity, high optical rotation and low impurity content.

The invention relates to a preparation method of a prothioconazole intermediate. The preparation method comprises the following steps: dissolving [1-(2-chlorophenyl)-2-(1-chlorocyclopropyl)-2-hydroxy]-propyl hydrazine into methyl benzene; dropwise adding a formaldehyde aqueous solution or a polyformaldehyde aqueous solution under 30 to 35 DEG C; then adding in thiocyanate after completion of dropwise adding; then dropwise adding hydrochloric acid or sulfuric acid aqueous solution; keeping warm and reacting for 50 to 70 minutes after completion of dropwise adding; directly using a reaction solution for follow-up reaction or filtering the reaction solution after cooling; thus obtaining the prothioconazole intermediate 2-(1-chloro-cyclopropyl-1-yl)-1-(2-chlorophenyl)-2-hydroxy-3-(1,2,4-triazolidine-5-thioketone-1-yl)-propane. Through optimization on a whole route, for example, reaction temperature, reagents, a feeding procedure and the like, of the preparation method, an after-treatment method is simple, three wastes such as waste gas, waste water and waste residues are few, the reaction time is shortened, the purity and the yield of a product are higher, and the preparation method is suitable for industrial production.

The invention relates to a method for preparing 2-amino-4,6-dichloro-5-formamido pyrimidine. The method comprises the following steps of: performing nitrosation on malonic acid diethyl ester and acetic acid serving as raw materials and sodium nitrite at first; then, performing reduction and formylation with formic acid in the presence of zinc powder to form formyl amino malonic acid diethyl ester; finally, performing condensation and cyclization with guanidine hydrochloride to produce 2-amino-4,6-dichloro-5-formamido pyrimidine; performing chlorination by using quaternary ammonium salt as a catalyst; fractionally performing hydrolysis under an alkali action to obtain a product. The method has easily-available raw materials, and is short in reaction time, simple in aftertreatment and high in hydrolysis selectivity; the cost is obviously reduced; the total yield is up to 74 percent and the purity of the product is up to 99.0 percent.

Production of 1-(3,5-2(2,2-dimethyl) methyl cyanide) benzyl pyrrodiazole is carried out by taking 3,5-2(2,2-dimethyl) ethyl-methyl) toluene (II) as raw material, synthesizing to obtain anatritra intermediate 3,5-2(2,2-dimethyl) ethyl-methyl) toluene bromide (III) and reacting with 1,2,4-triazanezole to obtain final product. It's simple and convenient, has less impurities and better product quality.

The invention relates to a bicyclol preparation method and an intermediate compound thereof. Concretely speaking, the invention relates to the preparation method of bicyclol which is 4,4'-dimethoxy-5,6,5',6'-bis(methy-lenedioxy)-2-hydroxymethyl-2'-methoxycarbonyl-biphenyl shown in a formula (1), and the intermediate compound thereof.

The invention provides a preparation method of chiral 5-difluoromethoxy-2-[[(3,4-dimethoxy-2-pyridyl)-methyl]-sulfinyl]-1H-benzimidazole (pantoprazole) and a sodium salt thereof. The method comprises the following steps: in an organic solvent, adding an organic alkali in the presence of a chiral titanium complex prepared from a diamide R,R or S,S-tartrate ligand, a metal titanium reagent and water, and oxidizing prochiral thioether of pantoprazole by a hydrogen peroxide oxidizer to obtain the corresponding pantoprazole containing rich single antipode. The method has the advantages of high enantioselectivity, mild reaction, simple after-treatment process, fewer procedure steps, low solvent consumption and low cost, and is very simple to operate.

The invention provides a method for producing a liquid fuel by using biomass. The liquid fuel is obtained by performing pretreatment, a pyrolytic reaction and a catalytic cracking reaction on the biomass. The biomass is composed of pine needles, bamboo wood, tung tree branches, ginger stems and leaves, Chinese toon branches, sweet potato seedlings, Enteromorpha prolifera, leftovers from a slaughterhouse and the like, wherein the pine needles, the bamboo wood, the tung tree branches, the ginger stems and leaves, the Chinese toon branches and the sweet potato seedlings contain volatile oil, grease, cellulose, lignin and the like; Enteromorpha prolifera contains a large amount of carbohydrates, proteins, crude fibers, fatty acids and the like; and the leftovers from the slaughterhouse are rich in grease. The above biomass raw materials are subjected to the pyrolysis reaction and the catalytic cracking reaction for sufficient conversion, and the obtained liquid fuel is excellent in combustion quality.

The invention discloses a preparing method of 5'-deoxyribonucleoside monophosphate, which comprises the following steps: (1) mixing 2'-deoxyribonucleoside, phosphorus oxychloride and trialkyphosphate to obtain a crude solution containing 5'-deoxynucleotide; (2) hydrolyzing the 5'-deoxynucleotide crude solution obtained from the step (1) in a solution with pH higher than or equal to 8.0 so as to an obtain hydrolysis liquid; (3) mixing an organic solvent, i.e. halogenated hydrocarbon, with the hydrolysis liquid obtained from the step (2), and extracting the mixture to obtain an organic phase and an aqueous phase; (4) condensing the aqueous phase to obtain a condensed liquid; and (5) placing the condensed liquid obtained from the step(4) at a temperature of 10-15 DEG C to obtain the solid 5'-deoxyribonucleoside monophosphate.

The invention discloses a process for preparing alkylphenol formaldehyde oligomer sulfonate. The process comprises the following steps of: adding alkylphenol and a catalyst into a reaction kettle, heating with stirring, dripping a formaldehyde solution or paraformaldehyde, continuously stirring, and raising temperature to reaction temperature, adding residual formaldehyde solution or paraformaldehyde, continuously reacting, and after reaction is finished, adding a sodium hydroxide aqueous solution to adjust pH of a reaction product to be 6.5 to 8.0 to obtain alkylphenol formaldehyde oligomer; and adding the alkylphenol formaldehyde oligomer into the reaction kettle, adding a solvent to dissolve, opening a stirrer, stirring and heating to 30 to 80 DEG C, adding a sulfonating agent, continuously reacting for 30 to 90 minutes, neutralizing a sulfonating product by using alkali until pH is 7 to 8, and evaporating to remove the solvent to obtain the alkylphenol formaldehyde oligomer sulfonate. The process has the advantages that alkylphenol and formaldehyde are used as raw materials, the process is simple, and industrialization is easy to realize.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of high-purity 4, 4-dichlorodiphenyl sulfone. The preparation method of the high-purity 4, 4-dichlorodiphenyl sulfone comprises the following steps: firstly, mixing molybdate, organic dicarboxylic acid and hydrogen peroxide, dropwise adding the mixture into a mixed solution of 4, 4-dichlorodiphenyl sulfoxide and a solvent for reaction, and after the reaction is completed, performing post-treatment to obtain the high-purity 4, 4-dichlorodiphenyl sulfone and residual filtrate; the residual filtrate is directly used for the next round of reaction after being layered; the molar ratio of the 4, 4-dichlorodiphenyl sulfoxide to the molybdate to the organic dicarboxylic acid to the hydrogen peroxide is 1: (0.01-0.05): (0.02-0.1): (1-3). The invention provides the preparation method of the high-purity 4, 4-dichlorodiphenyl sulfone, the catalyst is low in cost, the preparation steps are simple, the post-treatment steps are simple, the reaction residual filtrate is circularly and efficiently utilized, the purity is high, and the yield is high.

The invention provides a method for producing saxagliptin. The method comprises the following steps of: 1, providing a compound d; and 2, reacting the compound d, isopropanol and concentrated hydrochloric acid at the temperature of between 50 and 80 DEG C, and collecting the product to obtain the saxagliptin. Compared with the prior art, the method has the advantages that the compound d is directly converted into the target product, so that the reaction rate is greatly improved, the reaction yield is improved, the post treatment method is simplified, and industrial wastewater is greatly reduced.

The invention provides a preparation method of an eluxadoline intermediate compound, and concretely discloses a method for preparing (S)-2-tertbutyloxycarbonyl amino-3-(4-carbamyl-2,6-dimethyl phenyl) propanoic acid shown by a formula 11. The method comprises the following steps of Step I, obtaining a compound shown by a formula 4 through a compound shown by a formula 1; Step II, obtaining a compound shown by a formula 5 by the compound shown by the formula 4; Step III, obtaining a compound shown by a formula 6 by the compound shown by the formula 5; Step IV, protecting amino groups in the compound shown by the formula 6 to obtain a compound shown by a formula 9; Step V, performing selective hydrolysis on the compound shown by the formula 9 to obtain a compound shown by a formula 10; then, performing ammonolysis to obtain the compound shown by the formula 11. The process routes of the method use the fire-new design; intermediate compounds obtained by the reaction in each step are all synthesized for the first time; a method of firstly performing carbonylation and then performing asymmetrical reduction is used in the process routes; the asymmetrical reduction is realized in the later stage; the catalyst consumption is favorably reduced; the cost is reduced. The formulas are shown as the accompanying drawing.

The invention discloses ester compounds and a preparation method thereof. The invention provides the ester compounds represented by a formula 2, wherein R1 is C1-4 alkoxy or hydrogen, R2 is C1-4 acylamino or hydrogen, R3 is C1-4 alkyl, and R4 is C1-4 alkyl. The preparation method of the ester compounds represented by the formula 2 has the step that: a compound 4 and anhydride represented by a formula 5 are subjected to an acylation reaction, such that the eater compound 2 is obtained.