314results about How to "Gentle operation" patented technology

The invention discloses a preparation method of metformin hydrochloride. The preparation method is characterized by using dicyandiamide and dimethylamine hydrochloride as raw materials, feeding the materials in a mole ratio of (1:1)-(1:1.2), using N,N-dimethylacetamide or dimethyl sulfoxide 2-4 times dicyandiamide by weight as a solvent, and reacting for 4-8 hours at 140+/-5 DEG C to prepare a crude metformin hydrochloride product; recrystallizing the crude product with ethanol, regulating the pH value to be 5-6, decoloring the crystal, cooling the crystal to minus 10-0 DEG C while stirring, precipitating the crystal, obtaining a refined metformin hydrochloride product through filtering and drying, and recovering the solvent from filtrate. The qualified product has yield of 80-85% and high purity. The preparation method has the advantages that as the selected reaction solvent has a relatively high boiling point, the recovery rate of the solvent is high; the phenomenon of material surging can be effectively avoided, so that the preparation method has the advantages of mild reaction conditions, simplicity in operation and high safety.

The invention discloses a method for preparing a compound shown as the formula (I), which is characterized by comprising the following steps of: (1) carrying out hydroxyl protection on a compound shown as the formula (II) by using a first hydroxyl protecting group, and then, reacting with hydride to generate a compound shown as the formula (III); (2) carrying out hydroxyl protection on the compound shown as the formula (III) by using a second hydroxyl protecting group, and then, removing the first hydroxyl protecting group to obtain a compound shown as the formula (IV); (3) enabling the compound shown as the formula (IV) to carry out non-corresponding selective epoxidation reaction to generate a compound shown as the formula (V); (4) reacting the compound shown as the formula (V) with thecompound shown as the formula (VI) in a polar aprotic solvent to obtain a compound shown as the formula (VII); and (5) carrying out condensation, desilylation and oxidization on the compound shown asthe formula (VII) to generate the compound shown as the formula (I). In the general formulas of the compounds in each step, R1 is selected from naphthyl or any substituted naphthyl; R2 is selected from alkyl or benzyl of C1-C4; P is selected from hydroxyl protecting groups, such as 2-methoxyl propyl or p-methoxyl benzyl and the like; P' is a hydroxyl protecting group capable of resisting and removing P, such as benzyl; and X is selected from Cl, Br, I or benzyloxyl.

The invention relates to a method for catalysis-synthesizing 2,5-dicarbaldehyde by carbohydrate; carbohydrate is used as raw material, N,N-dimethylacetylamide is used as reaction medium, sodium bromide is used as additive, 5-hydroxymethylfurfural is dehydrated under acid catalysis, vandic salt is added as the catalyst, and air flows in under normal pressure to carry out oxidizing reaction, so as to synthesize 2,5-dicarbaldehyde; in the method, the reaction condition is mild, the raw materials and the catalyst are obtained easily, the method has high 2,5-dicarbaldehyde yield and the reaction process is easily operated.

The invention discloses a preparation method of polyene ether compounds. The method includes: organic small-molecule 4-dimethylamino pyridine (DMAP) is used as the catalyst, binary alkynyl compounds and binary hydroxy compounds are mixed with organic solvent, and the polyene ether compounds are obtained by using the click polymerization reaction of alkynyl-hydroxy. The polyene ether compounds comprise an inner unit indicated by formula (I). The polymerization step is showed in the formula (V), wherein n is larger than 1, and R1 and R2 are selected from organic groups. The method has the advantages that water and oxygen do not need to be removed during reaction, polymerization temperature is low, polymerization efficiency is high, and no metal residues exist in products; the prepared polyene ether compounds are high in steric regularity, good in machinability, and high in heat stability, degradability and aggregation-induced emission performance.

The invention provides a method for preparing soluble silicate with high modulus by gasified slag. The method comprises the following steps of (1) leaching the gasified slag by acid, and separating solid and liquid, so as to obtain the activated gasified slag and liquid phase; (2) performing desilicication reaction on the activated gasified slag and an alkaline solution of which the concentrationof hydroxyl ions is 1 to 5 mol/L at the temperature of 85 to 105 DEG C, and separating solid and liquid, so as to obtain the desilicication liquid and solid phase; (3) post-treating the desilicicationliquid, so as to obtain the soluble silicate with high modulus. Compared with the prior art, the method has the advantages that any silicon source does not need to be added, the sources of the raw materials are broad, the reaction conditions are mild, the process is simple, and the operation is easy; the quality of the prepared silicate is higher, the modulus is 1.5 to 2.5, the production cost islower, and the secondary solid and liquid pollutants are not produced; the reduction and recycling type efficient utilization of the gasified slag can be realized, and the economic benefit and environment benefit are obvious.

The invention discloses a preparation method for edaravone. The preparation method comprises a step of subjecting hydrazinobenzene and ethyl acetoacetate to a cyclization reaction under a solvent-free condition and action of an acid so as to prepare edaravone, wherein the usage amount of the acid is 0.02 to 10 equivalent of the molar weight of hydrazinobenzene. The preparation method provided by the invention has the advantages of mild conditions, fast reaction, safety, reliability, easy and convenient operation, low cost, almost quantitative completion of the reaction, capacity of obtaining a high purity (greater than 98%) crude product which accords with medicinal standards after simple recrystallization, and suitability for industrial production.

The invention relates to a high-temperature endurable active toughener powder used for epoxy resin, which comprises a general molecular structural formula as right, wherein -R1- is the diatomic linking group of aromatic series binary primary amine containing phenolic hydroxyl groups and -R2- is the diatomic linking group of aromatic series binary estolide molecule. The preparation method thereof comprises the steps of mixing the aromatic series binary primary amine, 2,2-Bis[4-(4-aminophenoxy)phenyl]propane and the aromatic series binary estolide with the mol ratio ranging from 1:1-5:2-6 in phenol solvent to react with each other at a temperature ranging from 100 to 150 DEG C for 5 hours and then pouring the obtained products into a precipitator stirred at a high speed to precipitate solid powder which is then filtered, washed, marinated, filtered and dried for preparing the high-temperature endurable active toughener powder for epoxy resin. The preparation method has the advantages of simple process and low cost, is environmental friendly, can finish the preparation process in universal equipment, and is applicable to industrial production.

The invention discloses an extracting process for a club fungi polysaccharide. The extracting process comprises the following steps: carrying out the pretreatment of raw materials, carrying out the hot water leaching, ultrasonic extraction or microwave extraction, and storing the extract after concentration, alcohol deposition, centrifugation and drying, wherein the hot water leaching method has moderate conditions and simple operation; and the ultrasonic extraction method and the microwave extraction method can save time and improve the extraction efficiency. The extracted club fungi polysaccharide has an inhibition rate of 70 percent for little white rat S-180 and Ehrlich carcinoma, and has the functions of improving the immunity, diminishing inflammation, easing pain, and the like.

The invention discloses to a method used for simultaneous preparation of phospholipid microtubule and vesicle using point-plane electrode electric field. The method is used for solving a problem that existing method is not capable of realizing simultaneous preparation of phospholipid microtubule and vesicle. The method comprises following steps: step 1, electrode cleaning; step 2, preparation of phospholipid dry membrane; step 3, assembling of a sealed preparation apparatus; and step 4, preparation of the phospholipid microtubule and vesicle, and obtaining of the phospholipid microtubule and vesicle. Advantages of the method are that: firstly, the method is capable of realizing simultaneous preparation of the phospholipid microtubule and vesicle using point-plane electrode electric field in a same system, form of the obtained phospholipid microtubule is good, yield is high, and phospholipid microtubule size is relatively large and uniform; and secondly, the length of the obtained phospholipid microtubule ranges from 200 to 1300 mum, and diameter ranges from 1 to 2 mum; and diameter of the obtained phospholipid vesicle ranges from 15 to 120 mum. The method is used for simultaneous preparation of the phospholipid microtubule and vesicle using point-plane electrode electric field.

The invention discloses a preparation method and an intermediate of ramelteon. The preparation method comprises the following steps: 1. deprotecting a compound (5) in an organic solvent to obtain a compound (6); 2. after condensing the compound (6) and a chiral resolution reagent, crystallizing to obtain an S type condensate crystal, and hydrolyzing under alkaline conditions to obtain an S type optical isomer compound (7) of the compound (6); and 3. reacting the compound (7) with propionyl chloride under alkaline conditions to generate the ramelteon (8).

The invention provides a method for preparing a beta-amino-carbonyl compound. Aldehydes, ketones and amines are directly mixed under the condition of synergetic catalysis of titanocene dichloride and a ligand, and react at room temperature to obtain the beta-amino-carbonyl compound, wherein the ligand is salicylic acid or salicylic acid derivatives or structural analogues thereof. According to the method, the catalyst used in the method is low in cost, nontoxic and stable and effective to air and water, the reaction condition is mild, a solvent is not needed, the operation is simple, and the atom economy is high.

The invention provides a method for processing fresh castanea mollissima packaged products. The method comprises the following steps: taking fresh deburred castanea mollissima, shearing notches on castanea mollissima shells by using scissors, drying the castanea mollissima through hot air for 30-60 minutes at temperature of 40-50 DEG C, shelling and peeling manually, soaking the castanea mollissima in 1-3ppm ozone water for 30-45 minutes; then blanching the castanea mollissima in a freshness retaining and color protecting liquid for 5-10 seconds at temperature of 80-90 DEG C, then instantly putting the castanea mollissima into the freshness retaining and color protecting liquid at temperature of 5-10 DEG C for carrying out ultrasonic treatment for 30-45 minutes, then refrigerating the castanea mollissima for 10-16 hours at temperature of 2-8 DEG C, then pre-freezing the castanea mollissima for 10-16 hours at temperature of -18 DEG C to -48 DEG C, and finally, drying the castanea mollissima for 48-72 hours till the content of water is 10-18%, and packing in vacuum under a clean environment and thus obtaining the fresh castanea mollissima packaged products. The products have good color, fragrance, taste and shape, can be stored and transported for 2 months at room temperature and sold by bulks in common farmers markets; the products are applicable to cooking and preparation in houses and commercial catering and secondary processing and sales of castanea mollissima food factories; by trial marketing, the fresh castanea mollissima packaged products are deeply favored by all consumers.

The invention discloses a synthetic method for adenine. Malononitrile and thiourea are employed as raw materials. The raw materials are subjected to a cyclization reaction under action of sodium alkoxide, and 4,6-diamino-2-sulfydryl pyrimidine. Then through three reaction routes, adenine is obtained. Though the method has many reaction steps, no refining or drying are needed for the product of each reaction step, the product can be used in the next reaction step, and the operation is simple. The raw materials are easily available, the prices are relatively low, the reaction conditions are mild, the operation is simple, the reaction steps are decreased, the reaction time is shortened, the overall reaction yield is high, and the synthetic method is suitable for industrial production.

The invention discloses a preparation method for 3-substituted trifluoromethyl indole. Various substituted acetanilides are taken as a reaction substrate with a medium to excellent reaction yield, excellent reaction chemical selectivity, and high area selectivity; another isomer (2-substituted trifluoromethyl indole) is monitored to be not detected in detection; the conditions are gentle; the substrate is wide in scope of application (wherein R is H or various electron-donating groups such as CH3, OCH3, SCH3 and the like, as well as various electron withdrawing groups such as NO2, Cl and the like, and Ar is various substituted benzene rings); the preparation method is simple and convenient in operation, relatively low in cost, less in side reaction, high in product purity, convenient in separation and purification, and suitable for large-scale preparation; and a product prepared by the preparation method has a very good application prospect in the biomedicine field.

The invention relates to a method for preparing a spherical carbon heavy metal adsorbent. The method is characterized by taking pentosan extracted by a bleached hardwood pulp alkaline method as a raw material and pure water as a solvent, and comprising the steps of after treatment at high temperature and high pressure under a hydrothermal condition, centrifugally separating so as to obtain a dark brown solid product, namely carbon spheres rich in acid oxygen-containing functional groups, washing the dark brown solid product for many times by distilled water and absolute ethyl alcohol till filtrate is clear, and drying in vacuum so as to obtain the spherical carbon heavy metal adsorbent. The method has the main characteristics that the pentosan extracted from a byproduct of pulping and papermaking is taken as the raw material and is environmentally friendly, cheap and easily available, water is taken as the solvent, the reaction needs no modifier and further oxidation, the adsorbent containing a large quantity of hydroxyl and carboxyl oxygen-containing functional groups is formed through dehydration, condensation, aromatization and carbonization, the adsorbent and metal ions can have chelation, and the adsorbent can be used as high performance adsorbent for adsorbing heavy metal ions like Pb(II) and Cd(II).The hydrothermal reaction adopted in the method has a simple operation process and the adsorbent is low in cost and has an excellent adsorbing effect.

The invention belongs to the technical field of the catalytic synthesis, and particularly discloses a CO (carbon monoxide)-promoted method for directly oxygenizing a hydroxylated aromatic compound by molecular oxygen. The method provided by the invention uses an aromatic compound as a substrate, uses a combined catalyst consisting of a supported precious metal catalyst and a heteroatom zeolite containing Ti, V, Cu or Fe or a polyoxometalate, and uses the mixed liquid of water and an organic solvent as a solvent; the CO (carbon monoxide) and O2 (oxygen) are put into the reaction system; and, under the promotion of the CO (carbon monoxide), the molecular oxygen directly oxygenizes the hydroxylated aromatic compound to prepare a corresponding phenol compound. The equipment and the process used by the method provided by the invention are simple; the separation of the target product is relatively easy; the reaction conditions are moderate; the system is environment-friendly; and thus the method is a green process route.