42 results about "N-methylpyrrolidine" patented technology

A porphyrin array exhibiting a large two-photon absorption property, and being linked with an acetylenic bond(s), represented by the following formulas:

wherein R₁ represents an alkyl or aryl group, M₁ represents a metal ion capable of serving as a core metal and forming a coordinate bond with Im, M₂ represents two protons or a metal ion incapable of forming a coordinate bond with Im, R₂ and R₃ represent a group selected from a porphyrin residue or porphyrin metal complex residue, a cyclic diimide residue, a dialkylviologen residue, a benzoquinone residue, an N-methylpyrrolidine-fullerene derivative residue and a ferrocene residue, Im is represented by Im₁ or Im₂:

(R₈ represents methyl or H), L₁ represents —(—C≡C—)_m— (m=1 to 3); n represents an integer of 1 or more; R₉ represents one of R₁, R₂, R₃ and Im.

The invention relates to a synthesis method of cefepime dihydrochloride that is a bacteriophage. 7-amin cethalosporanic acid (7-ACA) is used as starting material and reacts with hexamethyldisilane amine (HMDS) and iodotrimethylsilane (TMSI) first to obtain 7-ACA for protecting amino and carboxyl; then 7-ACA, amino and carboxyl of which are protected, reacts with iodotrimethylsilane and N-methylpyrrolidine to synthesize (6R, 7R)-7-amino-3-((1-methyl-1-pyrrolidine) methyl) cephalosporin-3-alkene-4-carboxylic acid hydrochloride (7-MPCA) through a one-pot method; 7-MPCA reacts with AE active ester to obtain a product of cefepime dihydrochloride through acidylation reaction and salifying reaction. Compared with the existing technical route, the synthesis method has the advantages that the process conditions are simple, the operation is convenient, the product yield is high, the product quality is stable, the method is suitable for the large-scale industrialized production, etc.

The invention provides a synthesis method of cefepime hydrochloride. The synthesis method comprises the following steps: taking GCLE (7-phenylacetamide-3-chloromethyl-3-cepham-4-carboxylic acid p-methyl-oxybenzyl ester) as a raw material; cutting a 4-site protecting group (p-methoxybenzyl) and enabling the 4-site protecting group to react with N-methylpyrrolidine (NMP); then cutting a 7-site protecting group through an enzyme method to obtain an immediate 7-amino-3-(1-methylpyrrolidine)methyl)-3-cepham-4-carboxylic acid hydrochloride (7-ACP); taking cheap and available methoxyiminoacetic acid mercaptobenzothiazole active ester (AE-active ester) and the 7-ACP to be subjected to 7-site acylation reaction, so as to finally prepare the cefepime hydrochloride. A route provided by the invention can be used for obtaining the high-yield and high-quality cefepime hydrochloride without a delta2 isomer. The synthesis method provided by the invention has the advantages of simple process, no harsh reaction conditions and the like and is very suitable for industrial production.

The present invention discloses a nano-scale ultra-fine analcime preparation method, wherein an alkali source, a silicon source, an aluminum source, water and N-methylpyrrolidine are adopted as reaction raw materials and crystallization is performed for 5-200 h under autogenous pressure and 140-200 DEG C hydrothermal condition to obtain the small grain nanometer analcime. According to the present invention, the obtained nano-scale ultra-fine analcime has characteristics of simple process, pure crystal phase, high crystallinity, large specific surface, low cost and the like, and has wide application prospects in ion adsorption and purification.

The present invention relates to a process for preparing key intermediates for cephalosporin antibiotics substantially free of undesired Δ² isomer. Thus, 7-aminocephalosporanic acid (7-ACA) is silylated with hexamethyldisilazane in cyclohexane at reflux temperature. (6R,7R)-3-[(Acetyloxy)methyl]-7-(trimethylsilyl)aminoceph-3-em-4-oic acid obtained is reacted with the mixture of N-methylpyrrolidine and trimethylsilyl iodide in cyclohexane, desilylated with isopropyl alcohol and treated with hydrochloric acid to obtain [6R-(6α,7β)]-1-[[7-Amino-2-carboxy-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-en-3-yl]methyl]-1-methylpyrrolidinium inner salt hydrochloride. [6R-(6α,7β)]-1-[[7-Amino-2-carboxy-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-en-3-yl]methyl]-1-methylpyrrolidinium inner salt hydrochloride is N-acylated with syn-2-(2-aminothiazol-4-yl)-2-methoxyimino acetic acid 2-benzothiazolyl thioester (MAEM) followed by treatment with hydrochloric acid to give cefepime dihydrochloride monohydrate.

The invention disclose a preparation method of an anion exchange membrane by using 4,4'-trimethylenedipiperidine (TMDP) as a cross-linking agent. The preparation method is implemented according to thefollowing steps: (1) dissolving chloromethylated polysulfone in 1-methyl-2-pyrrolidinone (NMP) at room temperature to obtain a colorless transparent chloromethylated polysulfone solution A; (2) adding a certain amount of 4,4'-trimethylenedipiperidine into the chloromethylated polysulfone solution A at room temperature, and carrying out stirring for 0.5-2 hours to carry out a cross-linking reaction on the 4,4'-trimethylenedipiperidine with the chloromethylated polysulfone to obtain a chloromethylated polysulfone solution B; (3) adding N-methylpyrrolidine into the chloromethylated polysulfone solution B at room temperature, carrying out stirring for 0.5-4 hours to carry out a quaternization reaction until the reaction is completed to obtain a membrane casting solution; and (4) completely deforming the membrane casting solution, pouring the membrane casting solution on a clean glass plate, carrying out film scraping by using a scraper, then carrying out vacuum drying, soaking the glass plate in deionized water so that a membrane naturally falls off from the glass plate, and carrying out washing with deionized water to obtain the anion exchange membrane. The anion exchange membrane has good alkali resistant stability and swelling resistance.

The invention discloses a method for preparing N-methylpyrrolidine through catalysis. According to the method, 1,4-butanediol and a methylamine water solution which are used as raw materials react inan H2 reduction atmosphere at the reaction temperature of 230-330 DEG C and under the pressure of 4-10 Mpa for 1-8 h with a supported bimetal oxide as a catalyst to produce N-methylpyrrolidine. A supporter of the catalyst is an Al2O3, SiO2 or ZSM-5 molecular sieve, and active components are CuO and NiO. The method has the advantages that the reaction time is short, the catalyst is low in cost andreusable, the product yield is high and the like.

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 of the 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.

The invention relates to a measurement method of N-methylpyrrolidine content of cefepime dihydrochloride material and relative agent, for evaluating the quality of cefepime dihydrochloride material and relative agent. The invention discloses a liquid chromatograph which comprises using carboxylic cationic column as analysis column, uses a conductive detector to check, preparing flow phase, preparing sample solution and reference substance solution, using test method to respectively inject the sample solution and reference substance solution into a liquid chromatograph, recording high pressure liquid chromatographs, and calculating the N-methylpyrrolidine content of the sample. The inventive chromatograph system has easy balance, short sample test time, better repeatability in preserved time, stable baseline, durable column, high quality of chromatograph peak of N-methylpyrrolidine, better repeatability, accurate, simple and reliable process.

The invention relates to a cleaning agent, in particular to a paint cleaning agent which is strong, powerful, economical, high-efficient, energy-saving, environment-friendly, novel and concentrated and a preparation method thereof. The paint cleaning agent is prepared by the following raw materials by weight percent: 15 to 25 percent of dimethoxy dipropylene glycol, 25 to 40 percent of N-methylpyrrolidine, 5 to 8 percent of ethanolamine, 20 to 30 percent of ethyl acetate, 5 to 10 percent of fatty acid ester, 15 to 25 percent of dimethyl ketone and 0.2 percent of fruity essence.

The invention relates to preparation of organic alkalis of medical and chemical raw materials, particularly to a N-methylpyrrolidine preparation method, which comprises: a) under the catalysis of potassium iodide, carrying out a mixed reaction on 1,4-dichlorobutane and methylamine aqueous solution in an ether solvent to obtain N-methylpyrrolidine, wherein the ether solvent can form a hydrogen bondwith methylamine, and the boiling point of the ether solvent is greater than the azeotropic point of methylamine and water in the mixed system. According to the invention, the preparation method hasadvantages of abundant raw material sources and simple synthesis process route, and does not require high-pressure reaction conditions so as to achieve advantages of equipment investment reducing, production management simplifying, comprehensive cost reducing, excellent economical efficiency and wide popularization prospect compared with the high-pressure method; and the experimental results showthat with the application of the method to prepare N-methylpyrrolidine, the preparation yield is larger than 88%, and the product purity is larger than 99%.

Provided are a device and method for separating N-methylpyrrolidine, water and tetrahydrofuran. The device comprises a crude product dehydration working section and a product refining working section. The crude product dehydration working section comprises a crude product intermittent column, a first condenser, a phase splitting tank, a backflow head and the like. The crude product intermittent column comprises a crude steaming column reactor and a crude steaming column. The product refining working section comprises a refining intermittent column, a second condenser, a transition cut fraction receiving tan and a product receiving tank. The refining intermittent column comprises a rectifying column reactor and a rectifying column located at the top of the rectifying column reactor. The crude product dehydration working section is communicated with the rectifying column reactor of the product refining working section through a crude product storage tank communicated with the crude steaming column reactor. A two-column intermittent rectifying process is adopted in the method, water and tetrahydrofuran are taken out through the crude product intermittent column, left raw materials are purified through the product refining working section, and high-purity N-methylpyrrolidine is obtained. The problems that a traditional device and technique are large in energy consumption, low in yield, high in production cost and troublesome in aftertreatment are solved.