11results about How to "High synthetic yield" patented technology

The application provides a method for synthesizing N,N-diethyl-2-hydroxyphenylacetamide and analogues thereof, and a reaction route of the method is as follows: the method comprises the following steps: 1) reacting a compound of formula (III) with a compound of formula (IV) in a solvent A under the action of a condensing agent and a base for a certain time to obtain a reaction solution containing a compound of formula (II); 2) adding a reducing agent to the reaction solution containing the compound of formula (II) obtained in step 1), and reacting for a certain time; the reaction is monitored, and after the reaction is completed, the solvent is spun dry, separated and dried to obtain a crude product of the compound of formula (I); 3) purifying the crude product obtained in step 2) to obtain a pure product of the compound of formula (I); wherein R1 and R2 are independently hydrogen, an alkyl group or an aryl group; and A is a substituted or unsubstituted aryl group or a heteroaryl group.

The invention discloses a synthesis method of a trifluoromethanesulfonate radical promoted amidino nickel complex. The preparation method comprises the following steps: reacting N, N '-dialkyl substituted amidino alkali metal salt with a nickel precursor, adding trifluoromethanesulfonate as an accelerant, and regulating the reaction rate and selectivity by utilizing the coordination effect of trifluoromethanesulfonate so as to efficiently prepare the amidino nickel complex. In the process, an ether compound is used as a solvent, the reaction is carried out at 0-70 DEG C for 1-48 hours, the reaction yield can reach 90% at most, and the product purity is gt; and 98%. The method has the characteristics of easily available raw materials, simplicity and convenience in operation, mild reaction conditions, good target product selectivity, high synthesis efficiency, convenience in post-treatment and the like, and has industrial application prospects.

The application discloses a green preparation method of 4,4'-difluorobenzophenone. The method uses 4,4'-difluorobenzene as raw material, potassium bromide as catalyst, acetic acid as solvent, and oxygen as oxidant, and 4,4'-difluorobenzophenone is generated in high selectivity through one-step oxidation under mild conditions. The application surprisingly finds that in the presence of potassium bromide, a new non-metallic catalytic oxidation system of potassium bromide / acetic acid / oxygen is used to realize high-efficiency and high-selectivity conversion of the C-H bond at the benzyl position. Compared with the traditional method, the application does not need to use a transition metal catalyst, does not need to use carbon tetrachloride and other materials damaging the ozone layer, and does not need to involve a dangerous intermediate such as a diazonium salt, the process route is short, the atomic economy is high, the product yield is high, the product purity is high, the catalyst is cheap and easy to obtain, and the application has excellent industrial application prospect and green chemistry characteristics.

This invention discloses a floating catalyst and its application in the synthesis of p-hydroxyphenylhydantoin. Copper and manganese co-doped nano-TiO2 hydrosol is loaded onto fly ash cenospheres to form a gel. The dried gel is sintered at 600-700℃ to obtain a floating catalyst with fly ash cenospheres as the support. Its chemical composition is: SO42- 2‑ / TiO2-CuO-Mn2O3 / fly ash cenospheres; its mass composition is: TiO2-CuO-Mn2O3 / 2 25%‑30%, CuO3%‑10%, Mn2O 3 6%–20%, S 0.02%–0.1%, fly ash cenospheres 50%–60%; its specific gravity is 0.6–0.90 g / cm³. 3 Specific surface area is 10-50 m² 2 / g; possesses solid superacid properties with an acid strength H0 ≤ -14.5; dissolves in acidic solvents to generate trace amounts of copper and manganese ions. The catalyst of this invention can float on the surface of aqueous solutions, solving the problem of separating solid catalysts from insoluble p-hydroxybenzylhydantoin products; it catalyzes the synthesis of p-hydroxybenzylhydantoin via two pathways, achieving a product molar yield of 68%-72%; it possesses photocatalytic functionality, allowing for the regeneration of catalysts that have lost surface catalytic activity; and it reduces the generation of organic pollutants at the source.

This invention discloses a one-pot method for preparing amidine-lanthanum complexes. Specifically, the lanthanum salt first reacts with an ether compound; the product, without separation, is then directly reacted with an N,N'-dialkyl-substituted amidine alkali metal salt to prepare the amidine-lanthanum complex in a one-pot process. The reaction yield can reach up to 90%, and the product purity is >98%. This invention features readily available raw materials, simple operation, mild reaction conditions, good selectivity for the target product, high synthesis efficiency, and convenient post-processing, making it promising for industrial applications.

This invention belongs to the field of enzymatic synthesis technology, specifically relating to a method for enzymatically synthesizing fucosylated novo-LNO series human milk oligosaccharide chains, comprising the following steps: using sialic acid-protected asymmetric branched oligosaccharide I as a substrate, firstly, fucosylation modification of the C3 branch site of the glycan chain is achieved through a fucosylation enzyme module; subsequently, galactose is introduced at the C6 branch end using a galactosylation enzyme module; finally, the sialic acid protecting group is removed by sialyl glycosidase to obtain the monofucosylated target product. By introducing sialic acid as a temporary protecting group into the asymmetric branched oligosaccharide I, the recognition of the reducing lactose and the internal LacNAc unit by fucosyltransferase is blocked, thereby selectively introducing fucose onto the non-reducing LacNAc / LNB unit, accurately constructing the branched structure.

The application belongs to the field of energy chemical industry, and relates to a nitrogen heteroanthraquinone compound, a preparation method thereof and application of the nitrogen heteroanthraquinone compound in a liquid flow battery. The nitrogen heteroanthraquinone compound has high solubility and high redox potential. The application also relates to application of the nitrogen heteroanthraquinone compound in the liquid flow battery. As a positive active material of an electrolyte of the liquid flow battery, the nitrogen heteroanthraquinone compound can realize high energy density, high voltage efficiency and long cycle life.

This invention relates to the field of all-silica molecular sieve preparation technology, and discloses a method for preparing an MFI topological structure all-silica molecular sieve, the MFI topological structure all-silica molecular sieve and its application, comprising: (1) mixing molecular sieve mother liquor, organosilicate, organic template agent and KOH to obtain a colloidal mixture; (2) subjecting the colloidal mixture to a crystallization reaction; (3) performing solid-liquid separation on the crystallization product obtained in step (2) to obtain a wet molecular sieve and a crystallization mother liquor; drying and calcining the wet molecular sieve to obtain an MFI topological structure all-silica molecular sieve; (4) optionally concentrating the crystallization mother liquor, and then returning to step (1) to provide the molecular sieve mother liquor. This method can obtain highly crystallized, fine-particle all-silica-1 molecular sieves, reduce the raw material cost of molecular sieve synthesis, and improve the economics of the new gas-phase rearrangement process technology.

The application discloses a crystal material based on a cadmium-viologen complex, a preparation method and application of the crystal material. II (Btybipy)Cl4; wherein Btybipy is a double 1-(thienyl)-3-methyl-4,4'-bipyridyl-1-onium. II The application is connected with a cadmium-viologen complex with chlorine as a counter anion to form a zero-dimensional crystal material. (Btybipy)Cl4 is a zero-dimensional structure, and has the advantages of simple synthesis method and convenient purification; the viologen compound is used as a nitrogen-containing ligand, the viologen ligand has good water solubility, is beneficial to crystallization of the crystal material, and improves a synthesis yield; the synthesized crystal material is sensitive to light and a solvent, can occur a photochromic phenomenon, and can be applied as an ion sensing material.

This invention discloses a method for preparing polymethylsilane. The method includes cutting and crushing metallic sodium to obtain sodium fragments; adding the sodium fragments to an organic solvent and heating to a molten state to obtain a mixture; stirring and cooling the mixture to obtain a sodium sand mixture; mixing dichloromethylsilane, tetrahydrofuran, and 15-crown ether-5 and then adding the mixture dropwise to the sodium sand mixture for reaction, followed by cooling, solid-liquid separation, and distillation. This preparation method obtains a sodium sand product with uniform particle size, high activity, and clean surface by rapidly cooling after high-temperature dispersion of metallic sodium in a specific organic solvent system. By adding tetrahydrofuran and 15-crown ether-5 to dichloromethylsilane, the single electron transfer rate of metallic sodium to dichloromethylsilane can be increased, the activation energy of the reaction can be reduced, and the reaction efficiency can be improved. Furthermore, the continuous dropwise addition saves reaction time.

This invention relates to the field of catalysts for the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime, and discloses a method for preparing the catalyst and the method for the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime. The method includes: mixing a molecular sieve mother liquor, an organosilicate, an organic template agent, and KOH to obtain a colloidal mixture; subjecting the colloidal mixture to a crystallization reaction; separating the obtained crystallization product into a solid-liquid mixture to obtain a wet molecular sieve and a crystallization mother liquor; drying the wet molecular sieve to obtain a raw molecular sieve powder; optionally mixing the raw molecular sieve powder with a binder, and then rotating it to obtain spherical particles; calcining the spherical particles, and then contacting them with an alkaline buffer solution containing ammonium salt, ammonia, magnesium salt, and bromide salt. This catalyst, when applied in fixed-bed or moving-bed reactions, enables long-cycle, continuous production of caprolactam with a high conversion rate of cyclohexanone oxime.