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

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 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..