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161results about How to "The reaction route is simple" patented technology

Synthesis method of high-grade intermediate R-1 of rosuvastatin calcium

The invention relates to a synthesis method of a high-grade intermediate R-1 of rosuvastatin calcium. The synthesis method comprises the following steps: condensing a compound 1 serving as an initialraw material with 2-mercapto-5-methyl-1,3,4-thiadiazole to generate a compound 2, oxidizing the compound 2 with hydrogen peroxide to obtain a compound 3, and carrying out Julia-Kocienski Olefination condensation reaction on the compound 3 and a compound 4 to obtain the R-1, wherein the compound 1 is (4R-cis)-6-chloromethyl-2,2-dimethyl-1,3-dioxolane-4-acetic acid tert-butyl ester, and the compound4 is pyrimidine aldehyde. The synthesis method has the advantages of simple reaction route, mild reaction conditions, cheap raw materials, high reaction selectivity and almost no generation of cis-isomers; the method avoids the use of a phosphine salt in the route, so the generation of a large-polarity byproduct triphenylphosphine oxide in the product is avoided; the cost for synthesizing a rosuvastatin calcium bulk drug is greatly reduced; and no cis-rosuvastatin calcium impurity is formed in a subsequent reaction, so the influence of the impurity on the medicine effect of rosuvastatin calcium is avoided, and the method has great significance for reducing the medication burden of residents.
Owner:NENTER & CO

Method for synthesizing pregabalin with isobutyl butanedinitrile as intermediate

The invention discloses a method for synthesizing pregabalin with isobutyl butanedinitrile as the intermediate. The method includes the steps of conducting the Knoevenagel condensation reaction on isovaleraldehyde and ethyl cyanoacetate in cyclohexane solvent with piperazine as the catalyst, conducting Michael addition on the product obtained in the first step and cyanic acid in alkaline alcohol solvent, conducting the decarboxylic reaction on the product obtained in the second step in isopropanol solvent under the heating condition to obtain the isobutyl butanedinitrile solvent, conducting hydrolysis on the intermediate under catalysis of cyanide hydratase AtNiTl, and conducting catalytic hydrogenation with raney nickel as the catalyst. According to the method, isoamyl aldehyde and ethyl cyanoacetate which are low in price and easy to obtain are used as raw materials, and the isobutyl butanedinitrile intermediate is obtained through the Knoevenagel condensation reaction, Michael addition and the decarboxylic reaction. The intermediate is then catalyzed, hydrolyzed and reduced through cyanide hydratase AtNiTl, and pregabalin is obtained. The reaction route is simple, the yield of each step of reaction is high, and therefore the final total recovery and purity of pregabalin are ensured.
Owner:TAICANG YUNTONG BIOCHEM ENG

Furanosyl modified 1,3,4-thiadiazole derivative and preparation method thereof as well as application of derivative as bactericide

The invention discloses a furanosyl modified 1,3,4-thiadiazole derivative and a preparation method thereof as well as application of the derivative as bactericide. The structural formula of the derivative CAU-2010-ZJ is as shown in a formula I. In the formula, R is acetyl, allyl, propargyl, methyl or ethyl; and R' is isopropyl, naphthaline, phenyl or phenyl having 1-2 substituted groups, wherein the substituted groups are halogen, methyl, methoxy, nitro, trifluoromethyl, or heptafluoro isopropyl. The preparation method comprises the following steps: carrying out a condensation reaction on a compound as shown in a formula II and N-substituted thiosemicarbazide so as to obtain thiosemicarbazone; and then carrying out a MnO2 ring-closing reaction so as to obtain a compound as shown in the formula I. The result of a bactericidal activity assay indicates that the compound CAU-2010-ZJ and a preparation thereof have good growth inhibition effect on sclerotium germs, eggplant early blight germs, gray mold germs, seedbed rhizoctonia solani germs, rice blast germs, asparagus stem blight germs, pythium germs, damping-off fungi, peanut black spot germs, white rot germs, tomato leaf mildew germs and watermelon anthrax. The formula I and formula II are as shown in the specification.
Owner:CHINA AGRI UNIV

Preparation method of vitamin A ester intermediate C15 and vitamin A ester

The invention provides a preparation method of a vitamin A ester intermediate C15 and vitamin A ester. The method comprises the following steps: carrying out a halogenation reaction and a cyclizationreaction on 3, 7-dimethyl-3-hydroxy-1, 6-octadiene as an initial raw material, carrying out a substitution reaction on the obtained product and triphenylphosphine or triester phosphite to prepare a corresponding Wittig reagent, carrying out a Wittig reaction on the Wittig reagent and 2-methyl-4-acetoxy-2-butenal, performing acidifying, hydrolyzing and acidifying the obtained product, and carryingout a substitution reaction on the hydrolyzed and acidified product and triphenylphosphine or triester phosphite to prepare C15. The vitamin A ester can be prepared by carrying out a Wittig reaction on the obtained C15 and 2-methyl-4-R3 substituent carbonyloxy-2-butenal. The method has the advantages of single reaction type, easy operation and realization of reaction conditions, safe and environment-friendly operation, simple post-treatment and low cost; and the reaction activity is strong, the reaction selectivity is high, the atom economy is high, and the target product yield and purity arehigh.
Owner:XINFA PHARMA

Phosphate compound containing 1,2,3-triazole ring as well as preparation method and application thereof

The invention discloses a phosphate compound containing a 1,2,3-triazole ring as well as a preparation method and an application thereof. The structural formula of the phosphate compound containing the 1,2,3-triazole ring is shown as a formula (I). According to the method for preparing the phosphate compound containing the 1,2,3-triazole ring disclosed by the invention, the raw materials are low in price and readily available, the reaction route is simple, and the phosphate compound containing the 1,2,3-triazole ring is high in herbicidal activity. The measurement result of the herbicidal activity plating method proves that the phosphate compound has strong effects of inhibiting growth of roots and stems of wheat and oilseed rapes. The pot experiment proves that the phosphate compound has a good effect of inhibiting growth of barnyard grass. The phosphate compound containing the 1,2,3-triazole ring has high plant growth regulation activity and high herbicidal activity during low concentration.
Owner:CHINA AGRI UNIV

Preparation method of 1, 1 '-ethylene-2, 2'-dipyridyl dichloride

ActiveCN112500411AOvercoming long reaction routesSimple processOrganic chemistryDichloroethanePtru catalyst
The invention discloses a preparation method of 1, 1 '-ethylene 2, 2'-dipyridyl dichloride, which comprises the following steps: by using 2, 2 '-dipyridyl and dichloroethane as raw materials and a solvent A or a solvent B as a solvent, carrying out cyclization reaction at 120-300 DEG C to obtain 1, 1'-ethylene 2, 2 '-dipyridyl dichloride, wherein the solvent A is selected from dichloroethane; thesolvent B meets the following conditions: (1) the solvent B does not chemically react with reaction raw materials or reaction products; 2, reaction raw materials of dichloroethane and 2, 2 '-dipyridylcan be dissolved; compared with the prior art, the method has the advantages of simple process, short reaction route and low cost, and is suitable for industrial production. The catalyst is added into the reaction system, so that the reaction rate can be remarkably increased, and the raw material conversion rate and the target product selectivity are improved.
Owner:NANJING REDSUN BIOCHEM CO LTD

Method for synthesizing pregabalin

The invention discloses a synthesis method of pregabalin. The synthesis method comprises the following steps: carrying out addition elimination reaction on isovaleraldehyde and diethyl malonate in a solvent composed of DMSO (dimethyl sulfoxide) and carbon tetrachloride by using vanadium tetrachloride as a catalyst; carrying out Michael addition on the product obtained in the first step in an alkaline alcohol solvent; carrying out hydrogenation reaction on the product obtained in the second step with hydrogen gas by using a carbon-supported Pd catalyst; carrying out hydrolysis reaction on the product obtained in the third step in hydrochloric acid; and carrying out chiral resolution on the product obtained in the fourth step in an alcohol-water mixed solvent by using L-malic acid as a resolving agent. The cheap and accessible isovaleraldehyde used as the raw material is subjected to addition elimination, Michael addition, hydrogenation reaction, hydrolysis and chiral resolution to obtain the pregabalin. The method has the advantages of simple reaction route and higher yield of each step, thereby ensuring the total yield and purity of the final pregabalin.
Owner:TAICANG YUNTONG BIOCHEM ENG

Synthesis method of picolinafen

InactiveCN107382847AThe reaction route is simpleReaction conditions are easy to reachOrganic chemistryTrifluoromethylPhenols
The invention provides a synthesis method of picolinafen. The synthesis method comprises the following steps: reacting 2-chloro-6-trichloromethyl pyridine (formula II) with 3-trifluoromethyl phenol (formula III) to generate 2-(3-trifluoromethylphenoxyl)-6-trichloromethyl pyridine (formula IV); converting 2-(3-trifluoromethylphenoxyl)-6-trichloromethyl pyridine (formula IV) into 2-(3-trifluoromethylphenoxyl)-6-pyridine formyl chloride (formula V); and reacting 2-(3-trifluoromethylphenoxyl)-6-pyridine formyl chloride (formula V) with 4-fluoroaniline to generate picolinafen (formula I). By synthesizing a key intermediate namely 2-(3-trifluoromethylphenoxyl)-6-trichloromethyl pyridine (formula IV), the reaction route is well simplified, moreover, the reaction conditions can be reached easily, the product yield is high, and the synthesis method has a good value for scientific research and can be used in industry.
Owner:南通嘉禾化工有限公司 +1
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