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

The invention discloses a making method of organic silicon compound with little-surface tension quaternary ammonium group, which is characterized by the following: reacting (RO)2CH3Si(CH2)3X and secondary amine to produce organic silicon compound with tertiary amino; reacting with halogenated alkyl to do quaternised reaction; making the organic silicon compound with structure as (RO)2CH3Si(CH2)3N+R1R2R3X-; fitting for surface activator of organic silicon cation, sterilizer and antibacterial agent; lengthening sterilizing time.

The invention discloses an oleanolic acid oxime ester derivate compound, a preparation method and an application thereof. The structural formula of the compound is shown in formula I, and in the formula I, R refers to furyl, pyridyl, 1-menaphthyl, 4-chlorophenoxy methyl or phenyl with 1 to 2 substitutional groups; and the substitutional groups in phenyl with 1 to 2 substitutional groups are halogen (such as fluorine, chlorine, bromine and iodine) or nitryl. The preparation method comprises the following steps: 1) performing the esterification reaction between oleanolic oxime subject to benzylation protection and substituted carboxylic acids to prepare an oxime ester compound; and 2) removing benzylation protection on the oxime ester compound by Pd/C-H2 to prepare the compound in the formula I. The bactericidal activity test result shows that CAU2012-A has a favorable effect of inhibiting growth of sclerotinia scleotiorum, phytophthora melongenae, botrytis cintrea, pyricularia grisea, rhizoctonia solani and cotton fusarium wilt.

A process for preparing 2-amino pyridine and its alkyl derivative from 2-cyanopyridine or its alkyl derivative includes incomplete hydrolysis and Hofmann degradation. Its advantage is high output rate (80%) and purity up to 99% or more.

The invention discloses a method for preparing difluoroacetyl fluoride from 1-C1-C8-alkoxy-1,1,2,2-tetrafluoroethane as a raw material by gas-phase catalytic cracking reaction in the presence of an aluminum fluoride catalyst. According to the disclosed preparation method, the reaction route is concise and efficient, fewer by-products are generated, catalytic activity is high, catalyst stability ishigh, and industrial production is facilitated.

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.

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.

The invention provides a class of compounds with novel 5-oxime ester B2a structures, preparation methods of the compounds and applications that the compounds are used as insecticides, acaricides and nematicides. Structural formulae of the compounds are represented as a formula I, a formula II or a formula III. According to the invention, the structure of B2a, a byproduct of avermectin productive process, is optimized; a series of 5-oxime ester B2a compounds with novel structures is designed and synthesized; comprehensive insecticidal activity determination is performed on the compounds; and compounds with good pesticide effects are found. The reaction route is simple; the products have good insecticidal activity; the biological activity ratio of most compounds surpasses a control insecticide avermectin; and the biological activity increases obviously, and therefore, the compounds provided by the invention have very high pesticide researching value.

The invention provides a method for preparing dichlorohydrin through glycerinum chlorination under catalysis of an HY type molecular sieve. According to the method, dichlorohydrin is prepared by taking a biodiesel byproduct glycerinum as a raw material, a normal hydrogen chloride gas as a chlorinating agent and the HY molecular sieve of different silicon-aluminum ratios as chlorination catalysts by using a gas-liquid two-phase method. The method for preparing dichlorohydrin is low in raw material cost, relatively gentle in reaction condition and small in amount of byproducts, the catalyst HY molecular sieve is high in catalysis activity and good in selectivity, appropriate reaction conditions are selected, and the yield of dichlorohydrin is greater than 87%. In addition, after the catalyst is repeatedly used for 5 times, the yield of dichlorohydrin is still greater than 80%, and the circulation effect is relatively good. By adopting the method, a novel way is provided for industrial production of dichlorohydrin through glycerinum chlorination.

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.

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.

The invention discloses a method for preparing dimethyl furan-2,5-dicarboxylate by oxidizing and esterifying 5-hydroxymethyl furfural. The method comprises the following steps: using air and/or oxygenas an oxidant and using methanol as a solvent and a reactant without adding alkali or bromine; using a gold-based catalyst for catalyzing oxidation and esterification of 5-hydroxymethylfurfural to synthesize dimethyl furan-2,5-dicarboxylate. The method provided by the invention has high selectivity for dimethyl furan-2,5-dicarboxylate, and can ensure that a conversion rate of 5-hydroxymethyl furfural is greater than 95% and the selectivity of dimethyl furan-2,5-dicarboxylate is greater than 99%.

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.

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.

The invention relates to a 7-oxo-diazabicyclo [3, 2, 1] octane derivative compound, a preparation method thereof and an application, and belongs to the technical field of drug synthesis, and aims to solve the problem of how to obtain high-activity antibacterial drugs. The method includes the steps: performing condensation reaction of a compound in a formula IV and RH to obtain an intermediate product compound in a formula V in the presence of acid-binding agents; removing benzyl by hydrogenation deprotection treatment and then performing sulfonation or phosphorylation reaction to obtain the 7-oxo-diazabicyclo [3, 2, 1] octane derivative compound in a formula I. The RH is selected from substituted or unsubstituted 1H-1, 2, 3-triazole or 1H-1, 2, 4-triazole compound, and compounds in the formula VI or VII are in one-to-one correspondence to R2, R3 and R4 in the compound in the formula I. The derivative compound has good antibacterial activity and particularly has good inhibiting effects on pseudomonas aeruginosa and Escherichia coli, the method is simple in operation, and conditions are mild.

The invention discloses a production process of pradaxa mesylate. The production process comprises the following steps: (1) preparing an intermediate PR-I; (2) preparing an intermediate PR-II; (3) preparing pradaxa PR-III; (4) refining the pradaxa PR-III; and (5) preparing pradaxa mesylate. The production process is mild in reaction condition, simple in reaction route, convenient in operation, high in selectivity, and capable of shortening the production period; and the obtained pradaxa intermediate is low in water content, the prepared pradaxa mesylate is high in yield and purity, and the maximum impurity is low in impurity content; and the production process is less in emission of three wastes, environmentally friendly, free from requiring the columnar chromatography purification, suitable for the industrialized production, capable of avoiding the requirement of palladium-on-carbon high-pressure hydrogenation on equipment and capable of reducing the risk.

The invention discloses a preparation method of 2-piperidinecarboxylic acid, 3-piperidinecarboxylic acid and 4-piperidinecarboxylic acid. The method is as follows: 2-pyridinecarboxylic acid, 3-pyridinecarboxylic acid and 4-pyridinecarboxylic acid are used as the raw material respectively, hydrogen is used to reduce the raw material to the corresponding piperidinecarboxylic acid in the presence of palladium-carbon catalyst. The method has the advantages of simple route, less side reactions, low hydrogenation pressure and hydrogenation temperature, short hydrogenation time and simple treatment of solid wastes, and is easy to realize industrialization.

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.