18 results about "Chrysanthemic acid" patented technology

The invention belongs to the field of organic synthesis, and particularly relates to an efficient method for preparing ethyl chrysanthemate by using a Beta / CuCl nano molecular sieve catalyst. Glycine ethyl ester hydrochloride and sodium nitrite react in a heptane solvent to generate ethyl diazoacetate, and then ethyl diazoacetate reacts with octa-carbene to generate ethyl chrysanthemumate. The catalyst provides an acidic environment and active sites, promotes generation of diazo compounds, controls reactant diffusion through a pore channel structure, and improves the reaction rate and selectivity. The catalyst stabilizes the carbene intermediate and reduces the reaction temperature. The catalyst can be recycled, and environmental pollution and cost are reduced. The yield of the ethyl chrysanthemate exceeds 98%, the yield and quality are improved, and a new scheme is provided for the sanitary insecticide and pharmaceutical industry.

The application discloses a kind of carolic acid and preparation method thereof, and specifically relates to the field of medical technology.The method comprises the following steps: stirring catalyst H2WO4 / C with hydrogen peroxide, then adding dichloro chrysanthemic acid ethyl ester; oil bath heating is carried out, reaction temperature is controlled, repeated reflux is carried out, and oxidation reaction is carried out; after the reaction, homogeneous transparent solution is filtered, extracted, and subjected to reduced pressure distillation to obtain carolic acid product.In the application, when catalyzing and oxidizing dichloro chrysanthemic acid ethyl ester, a high-activity H2WO4 / C heteropoly acid is used as a catalyst, the reaction scheme is optimized, the selectivity of the reaction is greatly improved, the number of cycles of the catalyst is increased, and after 20 cycles of the new catalyst, the catalyst activity does not decrease obviously.Furthermore, due to the great improvement of selectivity, the loss of product is reduced, and the yield is improved.

The invention discloses a syringate compound capable of preventing and treating barn pests as well as a preparation method and application of the syringate compound. The syringate compound has the following molecular structure expression, and according to the design, the light stability is enhanced by utilizing a rigid cyclic structure of chrysanthemic acid, and the CarE activity can be inhibited through a propenyl side chain of eugenol, so that self metabolism inactivation of pyrethrin is blocked; .

The invention discloses a saussurea involucrata polypeptide and application thereof, and belongs to the technical field of polypeptides, the saussurea involucrata polypeptide comprises saussurea involucrata tripeptide-1, saussurea involucrata pentapeptide-4, saussurea involucrata tripeptide-5, saussurea involucrata hexapeptide-8, saussurea involucrata hexapeptide-9 or saussurea involucrata acyl snake venom tripeptide, and the saussurea involucrata polypeptide is prepared through an amide condensation method of saussurea involucrata acid. The invention has the following beneficial effects: the anti-wrinkle, firming, soothing and anti-oxidation effects of the thousand-day chrysanthemum acyl tripeptide-1, the thousand-day chrysanthemum acyl pentapeptide-4, the thousand-day chrysanthemum acyl tripeptide-5, the thousand-day chrysanthemum acyl hexapeptide-8, the thousand-day chrysanthemum acyl hexapeptide-9 or the thousand-day chrysanthemum acyl snake venom tripeptide have obvious effects on the anti-wrinkle, firming, soothing and anti-oxidation effects; particularly, the instant wrinkle removal effect is particularly outstanding.

The application discloses an esterase whole cell catalyst and preparation and application thereof, the esterase whole cell catalyst can express a carboxylic acid esterase mutant disclosed in the application, the carboxylic acid esterase mutant is subjected to the following mutations on the amino acid sequence shown in SEQ ID NO. 1: the glycine at the 236th position is replaced by valine, the arginine at the 417th position is replaced by phenylalanine, and the threonine at the 545th position is replaced by alanine. The application effectively solves the problems of low catalytic activity of a warming catalyst for resolving methyl chrysanthemate and poor product tolerance in the prior art. The esterase whole cell catalyst of the application significantly improves the activity of selectively resolving methyl chrysanthemate to prepare dextro-trans chrysanthemic acid, and the optical purity can reach more than 99%. Moreover, the carboxylic acid esterase mutant disclosed in the application can be expressed in a soluble form in cell supernatant, can be produced in a large scale through microbial fermentation, has mild reaction conditions, and is simple to operate, and is more suitable for industrial production.

The diazotization kettle comprises a kettle body and a kettle cover, two mounting pipes are fixedly mounted at the top of the kettle body, limiting mechanisms are arranged in the two mounting pipes, sliding grooves are formed in the tops of the two mounting pipes, clamping mechanisms are arranged in the two sliding grooves, and the clamping mechanisms are arranged in the two sliding grooves. Two second communication grooves, cavities and mounting grooves are formed in the kettle body, compression mechanisms are arranged in the two cavities, sealing mechanisms are arranged in the two mounting grooves, and extrusion mechanisms are arranged in the two second communication grooves. The kettle cover sealing device is reasonable in structural design, and through the arrangement of the sealing mechanism and the limiting mechanism, when a worker closes the kettle cover of the kettle body, the piston is driven to move through extrusion of the side wall of the kettle cover, so that the heat-resistant air bag is expanded, and a gap between the heat-resistant air bag and the kettle cover is filled and sealed; the kettle cover can be limited through the clamped limiting blocks, so that the kettle cover is prevented from shaking and falling off in high-strength reaction.

The invention discloses a diazotization process for producing ethyl chrysantheate, which is characterized in that the reaction ratio of glycine ethyl ester hydrochloride, water, sodium nitrite, water, glacial acetic acid and toluene is (480 + 660) kg: (262.5 + 660) kg: 36.8 kg: 800L, and comprises the following steps: S1, sequentially adding materials: sequentially adding tap water, glycine ethyl ester hydrochloride, acetic acid, toluene and a sodium nitrite aqueous solution into a diazotization kettle; wherein the sodium nitrite aqueous solution is added dropwise; according to the method, high-precision temperature control is performed on the sodium nitrite aqueous solution, so that the sodium nitrite aqueous solution is prepared efficiently and stably, uniform stirring is performed in a dropwise adding manner, the uniformity and the reaction rate of diazotization reaction are improved, sodium nitrite is dropwise added into acetic acid within a specified control range, the reaction stability of diazo liquid is enhanced, and the yield of the diazo liquid is increased. The cyclization reaction rate is improved.

The present invention discloses a novel pyrazole ester compound, the structural formula of the compound is shown in formula (I). The novel pyrazole ester compound of formula (I) described in the present invention has a novel molecular structure, and its chemical structural formula has distinct characteristics. In the structural formula, Q can be a common pharmacophore such as pyridyl, benzyl, chrysanthemic acid, pyrazolyl, thiazolyl, thienyl, oxazolyl, thiazolyl and pyrazole. Overall, the compound is an ester. The preparation method of the compound of formula (I) described in the present invention is simple, the raw materials are easily available, the reaction conditions are easily controlled, and the yield is high. The compound of formula (I) described in the present invention has obvious activity in inhibiting or killing agricultural harmful fungi and the effect of preventing and treating fungal diseases of crops, and has the purpose of being used as a pesticide bactericide.

The invention relates to the field of organic synthesis, relates to a method for splitting trans-2, 6-dimethyl-1-indene amine, and in particular relates to a method for obtaining (1R, 2S)-2, 6-dimethyl-1-indene amine by splitting trans-2, 6-dimethyl-1-indene amine by utilizing a chiral inulin compound. The method comprises the following steps: reacting a chiral inulin compound with trans-2, 6-dimethyl-1-indene amine under a heating condition to generate salt, cooling and crystallizing, and hydrolyzing the obtained solid under an alkaline condition to obtain (1R, 2S)-2, 6-dimethyl-1-indene amine. The chiral chrysanthemic acid compound is adopted as a resolving agent, a traditional amino acid derivative resolving agent is replaced, good durability and stability are achieved, and by optimizing resolving conditions and technological parameters, a universal solvent which is widely applied in the market, low in price and easy to obtain serves as a solvent system, and the resolution efficiency is improved. The resolution with high yield (greater than 97%) and high optical purity (ee value greater than 98%) is realized.

The present application relates to the composition containing the biologically effective amount of compound I and fluensulfamide or KII-9396, and the method for preventing and treating pests in agronomic and non-agronomic environment. The compound I has synergistic effect with fluensulfamide or KII-9396, can improve the pest control effect, reduce the application amount, reduce the use frequency, and reduce the use cost.

The invention discloses a desolventizing process for producing ethyl chrysantheate, which comprises the following steps: S1, stirring and desolventizing: opening a cyclizing liquid feeding valve and a vacuum tube valve of an efficient desolventizing tower, pumping a certain amount of cyclizing liquid into the efficient desolventizing tower in vacuum, closing the cyclizing liquid feeding valve and the vacuum tube valve, opening a manual emptying tube emptying valve to enable the interior of the efficient desolventizing tower to return to normal pressure, and then adding a catalyst into the efficient desolventizing tower; opening a gas phase feeding valve, a reflux valve and a circulating water inlet and outlet valve of the condenser of the efficient desolventizing tower; by adopting the three-stage desolventizing system, the removal of the 2, 5-dimethyl-2, 4-hexadiene can be divided into three stages for desolventizing, so that the 2, 5-dimethyl-2, 4-hexadiene with higher purity is separated from the cyclization liquid to the greatest extent, the recovered purity of the solvent and the 2, 5-dimethyl-2, 4-hexadiene is higher, the utilization rate of the raw material is improved, the 2, 5-dimethyl-2, 4-hexadiene is promoted to be recycled, and the yield of the 2, 5-dimethyl-2, 4-hexadiene is increased. The 2, 5-dimethyl-2, 4-hexadiene is low in impurity content, high in quality and capable of being directly recycled, and compared with conventional desolvation, the yield of the ethyl chrysanthemumate can be greatly increased.

The invention belongs to the technical field of novel pyrethrum compounds, and provides four insecticidal active compounds in pyrethrum flowers as well as a preparation method and application thereof. The insecticidal active compound provided by the invention has a structure as shown in the specification. The Tanacetute A and the Tanacetute B belong to lignan compounds, the Tanacetute C belongs to monoterpene ester compounds, and the Tanacetute D belongs to sesquiterpenoids. The TanacetumA-D enriches the variety of natural pyrethrin, shows remarkable insecticidal activity on aphids, especially on corn aphids, and is of great significance to development of novel biological insecticides. The invention also provides a preparation method of the insecticidal active compound provided by the technical scheme. The preparation method provided by the invention is simple to operate. According to the method, the pyrethrum flowers are used as raw materials for extraction, so that the resource utilization of the pyrethrum flowers is improved.

The present invention addresses the problem of providing an esterase which is useful for the production of (1R, 3S)-chrysanthemic acid. In esterase enzymes from microorganisms of the genus Arthrobacter, a plurality of amino acid substitutions are disclosed that are effective to increase reactivity, which is reactivity to ethyl (1R, 3S)-chrysanthemumate.

The present invention relates to the field of enzyme variants, and in particular, to Arthrobacter globiformis esterase variants suitable for the asymmetric hydrolysis of cyclopropane derivatives, specifically the pyrethric acid esters of any combination of four stereoisomers, for selectively obtaining (1R,3R)-pyrethric acid or a salt thereof. The present invention further describes an expression vector containing an Arthrobacter globiformis esterase variant, and a transformed host microorganism encapsulating the vector. The present invention further relates to the use of an Arthrobacter globiformis esterase variant for selectively obtaining (1R,3R)-pyrethric acid. In a further aspect, the present invention relates to the use of an Arthrobacter globiformis esterase variant for the asymmetric hydrolysis of a racemic cyclopropane derivative having at least two chiral stereocenters, for the asymmetric hydrolysis of a racemic cyclopropane derivative having at least two chiral stereocenters.

The present application relates to a kind of composition containing fluorine mite double ether or KII-9396 and its application.The compound I has synergistic effect with fluorine mite double ether or KII-9396, can improve pest control effect, reduce application amount, reduce use frequency, reduce use cost.

The present invention relates to the field of enzyme mutants, in particular Arthrobacter globiforme esterase mutants, which are suitable for asymmetric hydrolysis of any combination of four stereoisomers of cyclopropane derivatives, in particular chrysanthemic acid esters, to selectively obtain (1R, 3R)-chrysanthemic acid or a salt thereof. Expression vectors comprising the arthrobacter globiforme esterase mutants and host microorganisms transformed containing the vectors are also described. The invention also relates to an application of the arthrobacter globiforme esterase mutant in selectively obtaining (1R, 3R)-chrysanthemic acid. In further aspects, the present invention relates to the use of arthrobacter globiforme esterase mutants for the asymmetric hydrolysis of cyclopropane raceme derivatives having at least two chiral stereocenters, preferably for the asymmetric hydrolysis of cyclopropane raceme derivatives having at least two chiral stereocenters.

The present invention relates to a chiral ferrocene P,N,N-ligand with side arms, a synthesis method thereof and applications. Specifically: a ferrocenyl chiral amine and pyridine aldehyde (ketone) are reacted at room temperature in methanol, and then, NaBH 4 is added for reaction, and the chiral ferrocene amine-pyridine intermediate is obtained by column chromatography. Under nitrogen protection, the chiral ferrocene amine-pyridine intermediate is dissolved in anhydrous acetonitrile, a side arm substance such as benzyl bromide is added, and finally dry K 2 CO 3 is added, and the reaction is refluxed to obtain the chiral ferrocene P,N,N-ligand with side arms. The ligand synthesis method of the present invention has the characteristics of simple and easily available raw materials, mild reaction conditions, simple operation, etc. The catalyst prepared in-situ from the ligand and a copper metal precursor can efficiently and highly selectively catalyze the asymmetric cyclopropanation reaction of olefins, and is applicable to the asymmetric synthesis of chiral chrysanthemic acid, an important intermediate of the insecticide pyrethroid pesticides, with a yield of 80% and an enantioselectivity of 90%, and can be applied to industrial preparation.

The invention belongs to the technical field of bioengineering, and particularly relates to an enzyme-catalyzed condensation reaction method and application of the enzyme-catalyzed condensation reaction method in efficient synthesis of pesticides. The condensation reaction method comprises the steps that a biocatalyst containing an EstA enzyme mutant reacts in a reaction system containing substrates for enough time so as to convert the substrates into cypermethrin, the substrates are dichlorochrysanthemic acid and alpha-cyano-m-phenoxybenzyl alcohol, and compared with an amino acid sequence shown in SEQ ID NO: 1, the amino acid sequence of the EstA enzyme mutant is as shown in SEQ ID NO: 1, and the amino acid sequence of the EstA enzyme mutant is as shown in SEQ ID NO: 2. At least one position selected from the 148th position, the 298th position, the 300th position, the 301st position, the 303th position, the 304th position, the 312th position, the 314th position and the 315th position has a mutated amino acid sequence. Under preferable conditions, the yield of cypermethrin after 48 hours of reaction in the condensation reaction method provided by the invention reaches 96.62%, which is obviously superior to that of the currently reported condensation reaction method.