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31results about How to "Many side effects" patented technology

N,N-dimethyl tetrahydrofurfuryl amine synthesis method

The invention relates to organic compound synthesis methods, in particular to an N,N-dimethyl tetrahydrofurfuryl amine synthesis method. The method includes steps: 1) mixing reactants with N,N-dimethyl formamide or N,N-dimethylacetamide and formic acid in a reaction vessel, and performing heating reaction; 1) after heating reaction is finished, performing distillation recovery of DMF (dimethyl formamide) or DMAC (dimethylacetamide) and the formic acid, and subjecting residues to vacuum distillation to obtain N,N-dimethyl furfuryl amine which is an intermediate product; 3) subjecting the intermediate product N,N-dimethyl furfuryl amine to catalytic hydrogenation, and distilling to obtain a product of N,N-dimethyl tetrahydrofurfuryl amine. The N,N-dimethyl tetrahydrofurfuryl amine synthesis method has advantages that raw materials are cheap and extensive in source; problems of low furfural yield and difficulty in separation due to instability of furfural acids are avoided, and acidity and reducibility of the formic acid are fully used; high hydrogenation selectivity and catalyst recyclability are realized; mild conditions, easiness in implementation and high raw material utilization rate are realized, and excessive formic acid and N,N-dimethyl formamide or N,N-dimethylacetamide are easy to recover.
Owner:XIAMEN UNIV

Novel photochromic azobenzene compound and synthesis method thereof

The invention provides a novel photochromic azobenzene compound and a synthesis method thereof and relates to a novel compound N-[4-[2-(4-methoxyphenyl) diazenyl] phenyl]-2-nitroaniline with a photochromic property and a synthesis method of the novel compound. The synthesis method comprises diazonium coupling reaction and coupling reaction between aromatic amine and aromatic halides. According to the invention, coupling reaction conditions of aromatic amine and aromatic halides are very simple, to be specific, only alkali metal fluorides with equal molar mass are added into reaction liquid, and reflux is carried out at 130 DEG for 3 h; a solvent is not required to be subjected to anhydrous anaerobic treatment, that reaction is carried out under nitrogen or argon atmosphere is not required, no side reaction is generated, aftertreatment of the product is simple, the conversion rate is higher, the yield of the target product is 48-74%, in addition, equipment adopted by the invention is relatively simple, the cost is low, and obvious economic benefits and environment-protection benefits are realized. The defects, in the prior art, that coupling reaction between aromatic amine and aromatic halides can be carried out at high temperature, with existence of inorganic base and under anhydrous anaerobic inert atmosphere usually, the reaction time is long, side reaction is multiple and the yield is low are overcome.
Owner:HUBEI UNIV

Method for removing perfluorinated compounds (PFCs) in wastewater through micro-nano gas-floating coupled electrooxidation device

The invention relates to a method for removing perfluorinated compounds (PFCs) in wastewater through a micro-nano gas-floating coupled electrooxidation device. The method comprises the steps that (S1)a water inlet pump and a micro-nano bubble generation device are started, the gas inlet amount is adjusted to be 0.3-0.7 mL / min, and a milky gas-water mixture reaches a contact chamber of a reactiondevice through a high-speed water outlet diffuser; (S2) a stirrer is started, the pH value of the wastewater is adjusted through acid or base firstly through a chemical adding groove, and then a coagulant is added; (S3) the gas-water mixture reaches a separation chamber subsequently, the PFCs in the wastewater float upwards to the water surface under the effect of coercing and jacking of bubbles and the effect of a small amount of flocculant, and enter an electrooxidation unit from a slag-water mixture outlet, and the wastewater not containing the PFCs is discharged from a water outlet of a separation chamber; (S4) an electrolyte is added into the electrooxidation unit, after a collected PFCs water-slag mixture reaches a certain volume, the current density is adjusted for electrolysis, andpurified water is discharged from the water outlet; and (S5) the wastewater discharged from the water outlet finally enters a water outlet groove and is discharged after reaching the standard.
Owner:江苏智诚达环保科技有限公司

Preparation method of N-formyl cefotaxime

The invention discloses a preparation method of N-formyl cefotaxime, which is characterized by comprising the following steps: adding anhydrous formic acid into acetic anhydride, controlling the temperature at 25-35 DEG C, reacting for 30 minutes, cooling to 15 DEG C, adding cefotaxime acid in batches, heating to 35-40 DEG C, adding a metal catalyst to continue reacting when reactants start to agglomerate, reacting for 30 minutes, adding purified water, and reacting for 30 minutes to obtain N-formyl cefotaxime. And adjusting the pH value when white crystals are separated out, filtering and washing when the temperature is reduced to 10-15 DEG C, and drying at the temperature of 50-60 DEG C and the pressure of-0.085--0.095 Mpa until the water content is less than 2.5% to obtain a target product. According to the method, multi-step synthesis by taking 7-ACA as a raw material is not needed, the production cost is effectively reduced, the reaction steps are simple, the steps of phase inversion purification, carbon decoloration and the like are not needed, the operation is simple and easy to control, the weight yield can reach 80%, and the highest product purity can reach 98.6%. The method fills the blank of N-formyl cefotaxime impurities prepared by chemical synthesis, and has important theoretical significance and practical application value for improving the quality of cefotaxime sodium and reducing the clinical medication risk.
Owner:河北合佳创新医药科技有限公司

Process for producing 7-amino-3-[(1-methyl pyrrolidine) methyl]-3- cephalosporin-4-carboxylic dihydrochloride

The invention discloses a method for preparing 7-amino-3-[(1-methylpyrro-lidinio)methyl]-3-cephem-4-carboxylic acid dihydrochloride, which comprises the following steps: imidazole, trimethylchlorosilane and 7-ACA react in a methylene dichloride solvent at a temperature of between 10 and 30 DEG C, and then are filtered; the temperature is reduced, and TMSI is dripped to react; THF is added into the mixture after methylene dichloride is distilled from a reaction feed liquid, and a N-methylpyrrolidine solution is dripped and stirred at a temperature of between 30 DEG C below zero and 25 DEG C below zero to react; methanol is dripped after the reaction, and then concentrated hydrochloric acid or hydriodic acid is dripped to hydrolyze; a hydrolysate is added with the methylene dichloride, and an aqueous phase is obtained through the separation; a yellow aqueous solution is obtained after the aqueous phase is decolored; and then acetone is added into the mixture to be filtered, washed and dried to obtain a 7-MPCA product. The methylene dichloride is distilled, so as to effectively improve the utilization rate of equipment, and the method can improve 30 percent of the utilization rate ofthe equipment compared with a process that the methylene dichloride is not distilled; and imidazole hydrochloride generated by the reaction which affects the subsequent layering and crystallization is filtered, which is favorable for the reaction, and ensures that the yield can reach 100 percent and the purity of a liquid phase is more than 99 percent.
Owner:河北九派制药股份有限公司

A kind of n, n-dimethyltetrahydrofurfurylamine synthetic method

The invention relates to organic compound synthesis methods, in particular to an N,N-dimethyl tetrahydrofurfuryl amine synthesis method. The method includes steps: 1) mixing reactants with N,N-dimethyl formamide or N,N-dimethylacetamide and formic acid in a reaction vessel, and performing heating reaction; 1) after heating reaction is finished, performing distillation recovery of DMF (dimethyl formamide) or DMAC (dimethylacetamide) and the formic acid, and subjecting residues to vacuum distillation to obtain N,N-dimethyl furfuryl amine which is an intermediate product; 3) subjecting the intermediate product N,N-dimethyl furfuryl amine to catalytic hydrogenation, and distilling to obtain a product of N,N-dimethyl tetrahydrofurfuryl amine. The N,N-dimethyl tetrahydrofurfuryl amine synthesis method has advantages that raw materials are cheap and extensive in source; problems of low furfural yield and difficulty in separation due to instability of furfural acids are avoided, and acidity and reducibility of the formic acid are fully used; high hydrogenation selectivity and catalyst recyclability are realized; mild conditions, easiness in implementation and high raw material utilization rate are realized, and excessive formic acid and N,N-dimethyl formamide or N,N-dimethylacetamide are easy to recover.
Owner:XIAMEN UNIV
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