89results about How to "No need for recrystallization" patented technology

The invention provides a method for synthesizing tolfenpyrad, relates to a preparation method of the tolfenpyrad, and the method is used for solving the problems such as tedious process and poor product purity of an existing tolfenpyrad synthesis method. The method comprises the following steps of: 1, synthesizing ethyl propionyl pyruvate; 2, synthesizing ethyl 3-ethyl-5-pyrazolecarboxylate; 3, synthesizing ethyl 1-methyl-3-ethyl-5-pyrazolecarboxylate; 4, synthesizing ethyl 1-methyl-3-ethyl-4-chloro-5-pyrazolecarboxylate; 5, synthesizing 4-(4-methyl phenoxy) cyanophenyl; 6, synthesizing 4-(4-methyl phenoxy) benzylamine; and 7, synthesizing the tolfenpyrad. Since sodium ethoxide is replaced by sodium hydroxide, the method provided by the invention has the characteristics of short reaction time, no generation of isomer and high purity of the product; and the obtained product has high purity and does not need re-crystallization.

The present invention discloses a synthesis method of 3, 4-dihydro pyrimidine-2-alkone at the room temperature without a solvent. The synthesis method comprises the following steps: under the condition without a solvent, an aldehyde compound as shown in Formula (II), beta-dicarbonyl compound as shown in Formula (III) and a compound as shown in Formula (IV) are mixed for reaction with an acid catalyst at the room temperature, a TLC is used for examining the end point of the reaction, the filtered residue can be acquired through filtration after the reaction is completed, and the product as shown in Formula (I) can be acquired after the filter residue is washed and dried. The present invention has the advantages that the operation is simple, the yield rate of the reaction is high, the purity of the product is high, the process is conducive to the environmental protection, the product cost is low, and the present invention is suitable for industrial production.

The invention discloses a synthetic method of 3,4-dihydropyrimidin-2-one. In a condition without solvent and catalyst, an aldehyde compound of formula (II), a beta-dicarbonyl compound of formula (III) and an urea compound of formula (IV) are taken as raw materials, stirred and heated for 0.5-10h reaction at the reaction temperature of 80-150 DEG C, reaction solution is separated to obtain the 3,4-dihydropyrimidin-2-one of formula (I). In the whole process, only a little ethanol aqueous solution is used for washing, catalyst is not needed, a 'one pot synthesis' is used for preparation, and the operation is simple, thus avoiding the disadvantages of high energy consumption, serious pollution, high toxicity, inflammable and explosive properties and the like which are caused by the use of the solvent, and the method is environmentally friendly and suitable for the though of the green chemistry, and helps reduces the production cost.

The invention discloses a method for preparing 6-O-Beta-D-glucosyl-3,6,16,25-tetrahydroxycycloartane. The method comprises the following steps: inoculating pharmaceutical fungi in a solid culture medium containing Chinese traditional medicinal materials or residue thereof; fermenting under a certain fermentation condition; collecting the solid fermented material; and drying, pulverizing and extracting and separating to obtain the product. The method has the advantages that the process is simple, the waste reutilization is implemented, during the extracting and separating process, the macroporous resin method is not adopted to enrich the compound so that the repeated activation of the macroporous resin is obviated, the mixed n-butyl alcohol extraction solution is washed with sodium hydroxide solution to remove a great amount of phenolic acid impurities and color pigments, a neutral alumina chromatographic column is adopted for the purification so that the pigment impurities with the polarity similar to that of the target component is effectively removed so that the pure product can be directly obtained without need of the re-crystallization, the yield of the pure product is improved, and the method is worth extending and applying..

The invention discloses a method for preparing fenpropathrin. The method comprises the following: (1) a step of preparing mixed solution, which is to mix ether aldehyde, sodium cyanide aqueous solution, organic solvent and aminopyridine or derivatives thereof serving as a phase transfer catalyst so as to obtain the mixed solution; (2) a step of preparing a fenpropathrin-containing crude product, which is to add methyl cyanide acyl chloride dropwise to the mixed solution obtained in a step (1) at 10 to 20 DEG C, perform thermal insulation reaction for 3 to 6 hours at 20 to 40 DEG C and obtain the fenpropathrin-containing crude product; and (3) a step of refining, which is to layer the fenpropathrin-containing crude product obtained in a step (2), remove cyanide-containing wastewater layers, use water to wash oil layers to be neutral, remove the organic solvent and obtain fenpropathrin crude oil. The method can obtain the fenpropathrin crude oil with high purity, excellent color and high yield, is simple in separation, needs no recrystallization, avoids the production of waste mother liquor, and reduces production cost.

The invention discloses a method for preparing cyhalothrin, which comprises the following steps: (1) preparing a mixed solution as follows: mixing ether aldehyde, sodium cyanide water solution, organic solvent and aminopyridine or derivatives thereof as a catalyst to obtain the mixed solution; (2) preparing a crude product containing cyhalothrin: dropwise adding cyanuryl chloride to the mixed solution obtained in step (1) at the temperature of 0 DEG C-40 DEG C, and stirring after dropwise adding to obtain the crude product containing cyhalothrin; and (3) refining: layering the crude product containing cyhalothrin obtained in step (2), washing the oil layer with water, and removing the organic solvent to obtain the crude oil of the cyhalothrin. The method of the invention can obtain the crude oil of the cyhalothrin with high purity, good color and luster and high yield, has simple separation, does not need recrystallization, avoids the generation of discarded mother solution, and reduces the production cost.

The invention discloses a synthesis method of vinpocetine. The synthesis method comprises adding vincamine into a three-neck flask, adding toluene into the three-neck bottle, stirring the mixture in ice water bath, dropwise adding polyphosphoric acid, placing the mixture into oil bath after half an hour, installing a water separator and a condensation tube, pumping to be vacuum, replacingnitrogen for two times, and performing reaction for 8 hours at the temperature of 120 DEG C; drying solvent by distillation after reaction is finished, adding ethanol and water, simultaneously dropwise adding caustic soda solution, utilizing saturated potassium carbonate solution to regulate pH to be 12 when the pH is 9, separating out solid, filtering and performing vacuum drying to obtain apovincamine; and adding absolute ethyl alcohol into the three-neck bottle, stirring the mixture in the ice water bath for one hour, then adding caustic alcohol into the mixture, adding the apovincamine after half an hour's stirring, placing a reaction bottle in the oil bath, performing reaction for 12 hours at the temperature of 80 DEG C, then steaming out solvent, adding the solvent into hydrochloric acid, extracting the mixture through ethyl acetate, adjusting pH value of the water phase to 12, separating out solid, filtering and drying to obtain the vinpocetine. The synthesis method is few in reaction step, low in energy consumption and less in environment pollution, recrystallization is not needed, and the purity of the vinpocetine can reach 99.5%.

The invention provides a method for preparing vinylene carbonate through micro channel reaction. The method comprises the following steps: (1) preparing equipment, including an enhanced mass transfer micro channel reactor, a metering pump I, a metering pump II and a micro filter, wherein the enhanced mass transfer micro channel reactor comprises a preheater I, a preheater II, an ultrasonic device and a micro channel module; (2) uniformly mixing chloroethylene carbonate with an ester solvent so as to obtain a mixed liquid, synchronously inputting the preheated mixed liquid and triethylamine into a micro channel, heating, mixing, performing reaction, discharging a product obtained after the reaction is completed from a discharge valve, filtering so as to obtain a crude product, and rectifying the crude product into a rectifying still, so as to obtain the vinylene carbonate, wherein the mole ratio of the chloroethylene carbonate to the triethylamine is 1:(1.5-2.0). The method is simple, convenient and safe to operate, relatively small in quantity of byproducts, small in single solvent consumption, low in moisture content, relatively high in product purity and yield, small in environment pollution and applicable to industrial large-scale production, and continuous production can be achieved.

The invention relates to a preparation method of 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl, comprising the steps of adding 4,4'-bi(2-trifluoromethyl-4-nitrophenoxyl)biphenyl, an organic mixed solvent containing alcohols, and a catalyst in a high pressure reaction kettle, infusing hydrogen, stirring, substituting residual air, continuously infusing hydrogen, heating and raising temperature, reacting for 2-4 hours, cooling the reaction system to room temperature, slowly discharging pressure, and infusing nitrogen to substitute all residual air so as to ensure that the high pressure reaction kettle is in inert atmosphere, filtering, recovering filter residue, maintaining the mother liquid, condensing the mother liquid such that the solid content of the mother liquid is in the range of 40-80%, cooling, putting the mother liquid aside, separating out white crystal product, filtering, washing and drying to obtain 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl solid. The method has a simple technology, low cost, high purity and yield, and is environment-friendly and suitable for commercial production.

The invention discloses a method for preparing cyhalothrin, which comprises the following steps: (1) preparing a mixed solution as follows: mixing ether aldehyde, sodium cyanide water solution, organic solvent and aminopyridine or derivatives thereof as a catalyst to obtain the mixed solution; (2) preparing a crude product containing cyhalothrin: dropwise adding cyanuryl chloride to the mixed solution obtained in step (1) at the temperature of 0 DEG C-40 DEG C, and stirring after dropwise adding to obtain the crude product containing cyhalothrin; and (3) refining: layering the crude product containing cyhalothrin obtained in step (2), washing the oil layer with water, and removing the organic solvent to obtain the crude oil of the cyhalothrin. The method of the invention can obtain the crude oil of the cyhalothrin with high purity, good color and luster and high yield, has simple separation, does not need recrystallization, avoids the generation of discarded mother solution, and reduces the production cost.

The invention relates to a novel method used for preparing N-methyl moxifloxacin. According to the novel method, N-methyl moxifloxacin is obtained via direct methylation of moxifloxacin hydrochloride II. Starting materials of the novel method are cheap and easily available; reaction conditions are mild; and the object product can be obtained via one-step reaction. The novel method is used for preparation of moxifloxacin hydrochloride impurity comparison products, is capable of realizing effective quantification control of the impurities, and is beneficial for increasing of quality of moxifloxacin hydrochloride bulk drug and preparations.

The invention discloses an efficient purification device of plant extracts and a purification method of the plant extracts. The device comprises a purification tank and a drying cabinet, wherein the purification tank comprises a purification tank body, a purification tank cover, a solvent chamber and a filter plate, the solvent chamber is positioned on the periphery of the purification tank body and is fixed on the purification tank body, the purification tank body is separated from the solvent chamber by the filter plate, a liquid inlet tube and a liquid outlet tube are respectively arranged on the solvent chamber, the drying cabinet comprises a drying cabinet body and a cabinet door, a gas outlet is formed in the top of the drying cabinet body, a gas inlet tube is arranged at the bottom of the drying cabinet body, a sieve-shaped support plate is arranged on the lower part of the drying cabinet body, the drying cabinet body is divided into a purification tank placing chamber and a heating chamber by the sieve-shaped support plate, and a heat exchanger tube is installed in the heating chamber. According to the method, the purification device is utilized to purify the plant extracts by using chromatography, and a good effect is achieved. The purification device has the advantages of simple structure, convenience in use and low manufacturing cost. The method has the advantages of simple process flow and high purification efficiency, and the consumption of organic solvents is greatly reduced.

The invention relates to the medicine chemical engineering field, in particular to a method for purifying and refining glycyrrhetic acids from liquorices by microwave assistant cloud point extraction. The method is as follows: firstly, by the microwave assistant extraction method, glycyrrhetic acids are extracted from liquorices quickly and efficiently; secondly, cloud point extraction is made bya glue ball solution formed by nonionic surfactants, and the pH value is adjusted to between 1.5 and 3.0, and after the glue ball solution is heated to the cloud point temperature, the glue ball solution is divided into two phases of a water phase and a glue ball phase, and the glycyrrhetic acids are mainly in the glue ball phase; by taking water as a solution, the pH value of the mixed solution is adjusted to between 6.0 and 8.0, and the cloud point back washing is made again, finally the water phase solution containing abundant glycyrrhetic acids is obtained, and coarse glycyrrhetic acids are obtained after the acidification and precipitation of the water phase solution, and the ethanol with high concentration is added to coarse glycyrrhetic acids, after heat dissolution and filtering, the glycyrrhetic acid tripotassium salt is obtained; the glycyrrhetic acid tripotassium salt is added with and dissolved in glacial acetic acids, and is crystallized and separated out, and thus the white glycyrrhetic acid monopotassium salt with high purity is obtained, the purity of the glycyrrhetic acid monopotassium salt is more than 90 percent. The method has the advantages of simple operation, no volatile organic solvent in the process of extraction and high enrichment and purification efficiency.

The invention relates to a preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene, comprising the steps of adding 2,5-bi(2-trifluoromethyl-4-nitrophenoxyl)toluene, an organic solvent, and a palladium / carbon catalyst in a reaction kettle, heating the reaction kettle, stirring, raising temperature to 70-80 DEG C, dripping a hydrazine hydrate aqueous solution, strictly controlling thedripping time within 1-1.5 hours, reacting for 2-4 hours at 70-80 DEG C after finishing dripping the aqueous solution, filtering when the solution is hot, removing filter residues, maintaining the mother liquid, dripping deionised water into the mother liquid while stirring, putting the mother liquid aside for 5-8 hours, separating out white solid product, filtering, washing and drying to obtain2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene solid. The method has a simple technology, low cost, high purity and yield, and is environment-friendly and suitable for commercial production.

The invention relates to a method for preparing 4,4'-bis(4-nitro-2-trifluoromethylphenoxy)diphenylsulfone, which comprises the following steps: adding 4,4'-dihydroxydiphenylsulfone and 2-chloro-5-nitrotrifluoromethylbenzene into a reaction kettle; adding a salt forming agent, strong polar aprotic organic solvent and an organic entrainer, stirring the mixture in the reaction kettle at room temperature for 30 minutes, and heating the mixture for azeotropic water separation reaction for 12 to 15 hours; and filtering the hot solution, removing filter residue, concentrating mother solution, cooling and standing the mother solution to precipitate a milky crystal product, filtering the solution, and washing and drying the milky crystal product to obtain the 4,4'-bis(4-nitro-2-trifluoromethylphenoxy)diphenylsulfone. The preparation method has the advantages that: the operation is simple, the raw material resource is readily available, the cost is low, and no corrosive substance is related to or generated; few kinds of organic solvents are used, and the organic solvents can be used repeatedly and circularly and are environmentally-friendly; and the product has a high yield up to more than 98 percent, a purity up to 99.8 percent and a melting point of from 198.4 to 199.2 DEG C and is suitable for industrial production.

The invention discloses a method for preparing 6-O-Beta-D-glucosyl-3,6,16,25-tetrahydroxycycloartane. The method comprises the following steps: inoculating pharmaceutical fungi in a solid culture medium containing Chinese traditional medicinal materials or residue thereof; fermenting under a certain fermentation condition; collecting the solid fermented material; and drying, pulverizing and extracting and separating to obtain the product. The method has the advantages that the process is simple, the waste reutilization is implemented, during the extracting and separating process, the macro porous resin method is not adopted to enrich the compound so that the repeated activation of the macro porous resin is obviated, the mixed n-butyl alcohol extraction solution is washed with sodium hydroxide solution to remove a great amount of phenolic acid impurities and color pigments, a neutral alumina chromatographic column is adopted for the purification so that the pigment impurities with the polarity similar to that of the target component is effectively removed so that the pure product can be directly obtained without need of the re-crystallization, the yield of the pure product is improved, and the method is worth extending and applying..