15results about How to "Short synthesis cycle" patented technology

The invention relates to the field of drug synthesis, and discloses a method for preparing semeglutide through fragment condensation, which comprises the following steps: taking 1-4 amino acids of a semeglutide amino acid sequence as a fragment I, 1-16 amino acids of the amino acid sequence as a fragment II, 17-29 amino acids of the amino acid sequence as a fragment III, and 30-31 amino acids of the amino acid sequence as a fragment IV; preparing the first fragment, the second fragment, the third fragment and the fourth fragment into a semeglutide product by adopting a solid-liquid combination method; the fragment I of the method can effectively inhibit racemization impurities of His; the C-terminal amino acids of the second fragment, the third fragment and the fourth fragment in the method are all Gly, and racemization impurities cannot be generated when the three fragments are condensed. In addition, the fragment synthesized by the fragment II, the fragment III and the fragment IV is high in purity and good in solubility, the condensation reaction efficiency of the polypeptide fragment is high, the fragment utilization rate is high, the cost is low, the unutilized fragment can be extracted and separated, and the post-treatment is simple.

The invention belongs to the technical field of medicine synthesis, and particularly discloses a preparation method of esostine, which comprises the following steps: taking 2-aminobenzoic acid as an initial raw material, acylating with propionic anhydride, and cyclizing to obtain a compound 2; then reacting with o-aminophenetole and sodium hydroxide at high temperature to obtain a compound 3; oxidizing with hydrogen peroxide to obtain a nitrogen oxide compound 4; then reacting with methylsulfonyl chloride for chlorination to obtain a compound 5; reacting the compound 6 with single Boc piperidine, and then removing Boc protection to obtain a compound 7; and reacting the compound 5 with a compound 7 to obtain a compound 8, namely Erastatin. According to the method, polybrominated substituted impurities generated by bromination are avoided, the overall yield is increased, the product purity is high, and the Pd residue is less than 5ppm.

This invention relates to the field of flame retardant preparation technology, and more particularly to a method for preparing an environmentally friendly and highly efficient flame-retardant polyolefin cable sheath material. The invention uses compounds containing primary amino and amide bonds and compounds containing phenyl and phosphoryl chloride groups as raw materials. The reaction is carried out at room temperature for 0.5-1 h, then heated to 45 °C for 3-4 h, and then to 65 °C for 5-6 h. Through a condensation reaction, a phosphoramide macromolecular flame retardant containing phenyl and amide bonds is obtained, with a yield as high as 80.5-95.6%. This flame retardant is added to polyolefin cable sheath material at a mass ratio of 25%, then compounded and extruded to obtain a halogen-free flame-retardant polyolefin cable sheath material. The flame retardant molecule prepared by this invention simultaneously contains phosphorus and nitrogen flame-retardant elements and amide bonds forming a char skeleton. During combustion, it can exert a phosphorus-nitrogen synergistic flame-retardant effect and promote the catalytic char formation of the matrix, which can significantly reduce the heat and toxic gas release of polyolefin cable sheath material during combustion, thereby providing protection for the lives of people in fire scenes.

The application belongs to the field of pharmaceutical chemical industry, and particularly relates to a liquid-phase preparation method of a side chain of somatuline. The preparation method of the application is that Fmoc-His(Trt)-OH reacts with H-Aib-OtBu under the action of a condensing agent T3P to obtain Fmoc-His-Aib-OH. The preparation method provided by the application simplifies operation steps, can control monomer impurities below 0.05%, can control inferior isomer impurities below 0.01%, is short in a synthesis period, is low in cost, has few by-products, and is suitable for industrial production.

The application discloses low-density monolithic porous carbon and a microemulsion preparation method and application thereof, and relates to the field of foam carbon materials. The porous carbon material comprises a three-dimensional network structure formed by cross-linking and stacking of cavity carbon nanoparticles, and has a density of 0.16-0.35 g / cm 3 ; the phenolic resin is used as a precursor, the foaming agent, i.e., the microemulsion droplet of the imidazole compound, is used as a template, and a green solvent is used, and the monolithic porous carbon is obtained through a sol-gel reaction, drying and pyrolysis. The imidazole compound and the hydrophilic end of the foaming agent interact to form a flexible small-molecule interface film, reduce the interfacial tension and stabilize the emulsion droplet. The foaming agent is decomposed to form a cavity spherical structure during carbonization. The monolithic porous carbon has a developed porous structure and surface hydrophobicity, is beneficial to constructing a high-efficiency electrocatalytic reaction microenvironment, and is reflected in improving the surface reaction gas concentration and inhibiting excessive mass supply, so as to improve the electrocatalytic reaction selectivity. Based on the morphology, pore structure and surface properties, the monolithic porous carbon also has application potential in the fields of water purification and heat insulation and flame retardation.

The invention relates to the field of drug synthesis, and discloses a preparation method of semeglutide with a high fragment utilization rate, which comprises the following steps: taking amino acids from the first site to the sixteenth site of a semeglutide sequence as a fragment I, and taking amino acids from the 17th site to the 29th site of the semeglutide sequence as a fragment II; the 30th to 31st amino acids of the sequence of the semeglutide are used as a fragment III; a semeglutide product is prepared from the first fragment, the second fragment and the third fragment through a solid-liquid combination method, three fragments with C-terminal amino acids being Gly are preferably selected in the method, racemization impurities cannot be generated during condensation of the fragments, the synthesized fragments are high in purity and good in solubility, polypeptide fragment condensation reaction is easy to carry out, and the method is suitable for industrial production. The input amount of amino acid is only 1.5-2 times when the fragment is synthesized, the synthesized fragment does not need to be purified, the input amount of a carboxyl terminal fragment is only 0.95-1.05 times that of the amino acid fragment when the fragment is condensed, the fragment utilization rate is high, the cost is low, the unutilized fragment can be extracted and separated, and the post-treatment is simple.

The invention relates to an NITER-SiCf / SiC ceramic matrix composite material and a preparation method thereof. The preparation method comprises the steps of powder preparation, SiC fiber weaving, slurry impregnation and hot pressed sintering. The preparation method of the powder comprises the following steps: performing in-situ growth of an RE3Si2C2 coating layer on the surface of SiC powder through a molten salt method to obtain SiC coated RE3Si2C2 powder with SiC coated with RE3Si2C2; the molten salt method comprises the following steps: taking rare earth metal elementary substance powder or rare earth metal hydride as a raw material, mixing the raw material with SiC powder and molten salt, and synthesizing to obtain SiC (at) RE3Si2C2 powder of RE3Si2C2 coated SiC; the step of slurry impregnation comprises the following steps: mixing SiC (at) RE3Si2C2 powder with a mixed solution to prepare SiC (at) RE3Si2C2 impregnation slurry, and then immersing the SiC fiber woven body into the SiC (at) RE3Si2C2 impregnation slurry.

The invention discloses a preparation method and low-temperature application of a Te-doped tungsten niobium oxide / molybdenum niobium oxide heterojunction, and belongs to the technical field of secondary batteries. The preparation method specifically comprises the following steps: carrying out high-energy ball milling and alloying on WO3, Nb2O5 and Te2O5 to obtain amorphous Te-doped tungsten niobium oxide; the preparation method comprises the following steps: carrying out high-energy ball milling and alloying on MoO3, Nb2O5 and Te2O5 to obtain amorphous Te doped molybdenum niobium oxide; uniformly mixing and compacting the amorphous Te doped tungsten niobium oxide and the amorphous Te doped molybdenum niobium oxide, and performing discharge plasma sintering in an inert atmosphere to obtain the ceramic crystal Te doped tungsten niobium oxide / molybdenum niobium oxide heterojunction material. The Te-doped tungsten niobium oxide / molybdenum niobium oxide two-phase heterojunction material designed by the invention is relatively short in synthesis time, the synthesis period is shortened, the size of crystal grains is convenient to regulate and control, the crystallinity of the material is very good, the diffusion rate of lithium ions is greatly promoted by a heterojunction interface, the electron conductivity is improved by cooperating with Te doping, and the performance of the Te-doped tungsten niobium oxide / molybdenum niobium oxide two-phase heterojunction material is improved. The material can be used as a lithium ion negative electrode material with fast charging characteristic and good low-temperature performance.

The invention relates to the technical field of nanometer materials, in particular to a synthesis method of gold nanoclusters and application of the gold nanoclusters in food pigment detection.The gold nanoclusters are prepared with natural plant protein ginger protease containing sulfydryl and reducing amino acid as an exclusive template through the following steps that an enzyme solution and a chloroauric acid solution are prepared and mixed and stirred in proportion to form colloid; and adding NaOH to adjust the pH so as to unfold the protein structure, carrying out microwave treatment after constant volume and uniform mixing, cooling, and storing in a dark place. The ginger protease is innovatively selected as a template, microwave synthesis is adapted, the synthesis period is shortened, and the product performance is improved; the detection system is high in specificity, good in interference resistance, mild in reaction condition, simple and convenient to operate, suitable for rapid detection of target pigments in various foods, and high in application value.

The invention provides a rapamycin derivative with better anticancer activity and a preparation method of the rapamycin derivative. The tumor cell proliferation inhibition activity of the rapamycin derivative provided by the invention is obviously superior to that of a parent compound rapamycin and a clinical drug temsirolimus. The method for synthesizing the rapamycin derivative through lipase catalysis has the advantages of being mild in condition, high in selectivity and wide in substrate application range, solves the technical problems that in traditional chemical synthesis, hydroxyl needs to be protected / deprotected, the steps are tedious and the selectivity is poor, and provides an efficient and green synthesis path for large-scale preparation of the novel rapamycin derivative.

The application discloses a lignin carbon fiber-based microneedle electrode, which comprises a working microneedle electrode, a counter microneedle electrode and a reference microneedle electrode; the working microneedle electrode is a specific biological recognition interface constructed by depositing gold on a microneedle substrate, bridging through a mercapto-polyethylene glycol-carboxyl self-assembled molecular layer and covalently coupling H3Cit antibodies by using an NHS / EDC·HCl activation method; the microneedle substrate is prepared by the following steps: ball milling and ultrasonic dispersion of lignin carbon fibers in a dichloromethane solution of polylactic acid-glycolic acid copolymer to obtain a slurry, and injecting the slurry into a microneedle array mold and removing bubbles in vacuum. The application discloses a three-electrode sensor, which comprises a working electrode, a reference electrode and a counter electrode, and the working microneedle electrode is used as the working electrode. The application discloses an application of the three-electrode sensor in detection of H3Cit. The lignin carbon fiber-based microneedle electrode has regular arrangement and good mechanical properties, and can effectively recognize H3Cit.

This invention discloses a surface-modified 2-aminopurine carbon sphere material, its preparation method, and its application, belonging to the field of new materials. In this invention, the synthesized surface-modified 2-aminopurine carbon sphere material is used for the separation and enrichment of N-glycopeptides and exosomes, possessing the following advantages: 1. The preparation process is simple, with a very short synthesis cycle, saving significant time and labor; 2. The reaction raw materials are common, and no organic reagents are used as solvents during the reaction, conforming to the design principles of green chemistry to reduce or eliminate the use and generation of hazardous chemicals and processes; 3. The microstructure and size of the material can be continuously adjusted by optimizing the reaction time, temperature, and raw material concentration, thereby obtaining the material with optimal performance and greatly improving the separation and enrichment capabilities of glycosylated peptides and exosomes.

The invention relates to the technical field of chemical synthesis, in particular to a synthesis method and application of asymmetric 1, 10-phenanthroline. The synthesis method of the asymmetric 1, 10-phenanthroline, provided by the invention, comprises the following steps: reacting 8-aminoquinoline and crotonaldehyde under the acidic condition and the catalytic action of NaI to obtain an intermediate 1; carrying out oxidation reaction on the intermediate 1 under an acidic condition to obtain an intermediate 2; and reacting the intermediate 2 with phosphorus oxyhalide to obtain the asymmetric 1, 10-phenanthroline. According to the synthesis method of the asymmetric 1, 10-phenanthroline, through three-step efficient reaction, the synthesis period is short, the production efficiency is high, the used raw materials are easy to obtain and low in cost, a convenient and efficient synthesis means is provided for researchers, and the asymmetric 1, 10-phenanthroline modification method and substrate range are widened; meanwhile, the method is suitable for large-scale industrial production and meets the large demand of the market on the phenanthroline derivative.

The invention provides a medical intermediate synthesis system, which relates to the technical field of medical intermediate synthesis, and comprises a reaction kettle, a raw material feeding module, a catalyst adding module, a stirring module, a temperature control module, a pressure adjusting module, a product separation module, a tail gas treatment module, an online monitoring module and a control system, the reaction kettle adopting a novel corrosion-resistant alloy material and a special anti-sticking coating reduces the adhesion and residue of reactants and shortens the cleaning time of the reaction kettle, so that the effective reaction time is increased, the high-precision raw material feeding module and the catalyst adding module are arranged, the accurate proportioning and uniform dispersion of the reaction materials are ensured, and the production efficiency is improved. The reaction rate and the conversion rate are improved, side reactions are reduced, the synthesis period is further shortened, ideal reaction conditions can be rapidly achieved and stably maintained through the efficient temperature control module and the efficient pressure adjusting module, and the reaction process is further accelerated.

The invention discloses a triamino cage type macromolecular hydrogen bond organic framework material and a preparation method thereof, and belongs to the technical field of organic synthetic chemistry. The invention provides a simplified preparation method aiming at the defects of tedious steps and low yield caused by the fact that trichlorine cage type macromolecules are prepared through two-step reaction (firstly synthesizing an intermediate and then closing a ring) in the traditional method. The method comprises the following steps: firstly, reacting 1, 3, 5-tri (4-hydroxyphenyl) benzene with cyanuric chloride for 2-5 days through a room-temperature'one-pot method 'under the catalysis of organic base to directly synthesize trichlorine cage type macromolecules; and reacting the intermediate with ammonia water at 140 DEG C for 4 hours, washing and recrystallizing to obtain the target product triamino cage type macromolecular hydrogen bond organic framework material. According to the invention, the traditional two-step synthesis of trichlorine cage type macromolecules is simplified into one step, the step of separating intermediates is omitted, the process is simple, the condition is mild, and the total yield is up to 76.7%. The obtained material is clear in structure and has wide application prospects in the fields of molecular recognition, gas adsorption separation and the like.