330 results about "Phase synthesis" patented technology

The invention provides a solid-phase synthesis method of semeglutide, and belongs to the technical field of synthesis of medical intermediates, and the method specifically comprises the following steps: segmenting a semeglutide main chain into three shorter polypeptide fragments, namely a fragment 4, a fragment 5 and a fragment 2, which are 7-14 sites, 15-22 sites and 23-37 sites; and respectively synthesizing and then assembling fragments to obtain a target product. The method specifically comprises the following steps: a) synthesizing a 7-14 peptide fragment and a 15-22 peptide fragment, and assembling the 7-14 peptide fragment and the 15-22 peptide fragment into a 7-22 peptide fragment, namely a fragment 1; b) synthesizing a 23-37 peptide fragment, selectively removing a protecting group A11oc on Lys26, and connecting with a side chain to form a fragment 3; c) connecting the peptide fragment 7-22 with the peptide fragment 23-37, and removing a protecting group to obtain a crude product; and d) separating and purifying to obtain a finished product. According to the invention, the purpose of high-purity, high-yield and low-cost synthesis of the semeglutide bulk drug can be achieved.

The invention discloses a split intein and application thereof, the split intein comprises two independent peptide fragments: (a) an N-terminal fragment, the amino acid sequence of which is as shown in SEQ ID NO.1; (b) a C-terminal fragment or a variant thereof, the amino acid sequence of the C-terminal fragment is as shown in SEQ ID NO.2, and the amino acid sequence of the variant is as shown in SEQ ID NO.3 or SEQ ID NO.4. The split intein has splicing activity and excellent splicing rate, the application of the split intein can be widened, the number of amino acids of the C-terminal fragment or the variant thereof is small, and the split intein has remarkable advantages in protein purification, solid-phase synthesis and the like.

The invention provides a microneedle preparation for co-delivering photo-thermal nano-enzyme and elemene as well as a preparation method and application of the microneedle preparation. The preparation method comprises the following steps: firstly, preparing a novel photo-thermal nano enzyme Au (at) MoS2 through a two-step water phase synthesis strategy; benefited from the synergistic effect of the hybrid material, the nano-enzyme shows significantly enhanced near-infrared (NIR) photothermal effect, peroxidase-like (POD) activity and glutathione-like peroxidase (GSHOx) activity, and can effectively remodel the tumor microenvironment and destroy the redox steady state. Furthermore, photo-thermal nano enzyme, beta-ELE and hyaluronic acid are used as raw materials, and a novel soluble microneedle preparation is successfully prepared through a template method. The novel composite microneedle is in a sharp rectangular pyramid shape, growth of melanoma can be effectively inhibited through percutaneous delivery of photo-thermal nano-enzyme and beta-ELE, remarkable systemic toxicity is avoided, and an innovative strategy is provided for non-invasive, efficient and safe melanoma combined treatment.

According to the portable solid-phase synthesis reaction device, in the portable solid-phase synthesis reaction device, a support module comprises a synchronous belt lead screw nut; the motor driving module is installed on one side of the upper end edge of the support module to serve as a power source component for adjusting the size of the composite column cavity, the motor driving module comprises a stepping motor and a synchronous wheel, the synchronous wheel is installed on an output shaft of the stepping motor, and the synchronous belt is arranged on the synchronous wheel and the synchronous belt lead screw nut in a sleeving mode; the lead screw lifting module is installed on the column top support to serve as an execution component for adjusting the size of the composite column cavity and comprises a transmission lead screw, a piston unit is installed at the lower end of the transmission lead screw, and the transmission lead screw is in threaded connection with a synchronous belt lead screw nut. The synthesis column body module is mounted in the middle between a column top support and a bottom plate of the support module to serve as a synthesis carrier to be filled and a solid-phase synthesis reaction vessel, and the synthesis column body module comprises a synthesis column.

The invention discloses a hexapeptide TE6 with xanthine oxidase inhibitory activity and a preparation method and application thereof, and belongs to the technical field of small molecule peptides. The amino acid sequence of the hexapeptide TE6 is TIATVE, and the hexapeptide TE6 can be prepared through a solid-phase synthesis method and an enzymolysis method. The hexapeptide TE6 is identified from a solieria cavaleriei proteolysis solution and has potential interaction with xanthine oxidase, under the concentration of 0.1 mg / mL, the xanthine oxidase inhibition rate is 44.74%, and compared with goose carnosine (the xanthine oxidase inhibition rate is 36.03%), the xanthine oxidase inhibition rate is remarkably increased (plt; 0.05), which is stronger in xanthine oxidase inhibitory activity, and can be used for preparing a preparation for inhibiting xanthine oxidase activity and relieving hyperuricemia.

The invention provides a preparation method of an efficient selective antagonist BQ-788, and relates to the technical field of preparation of antagonists. A solid-liquid combination method is adopted for synthesis, due to the fact that dimethyl dialkanoate on a side chain of tryptophan (DTrp) is difficult, Fmoc-DTrp (CO2Me)-OH is obtained through liquid-phase synthesis, p-methoxybenzyl is selected for protecting carboxyl in the synthesis process, the carboxyl can be removed through trifluoroacetic acid subsequently, and the risk that an indole ring of tryptophan is reduced due to hydrogenation can be successfully avoided. According to the present invention, by using the solid phase synthesis method, the fragment can be rapidly and efficiently obtained, the racemization problem during the condensation process can be effectively avoided, the urea is formed on the solid phase, the operation is simple and convenient, the hydrogen and the diphosgene are not used during the preparation process, the production is safe, the obtained product has characteristics of high yield and high purity, and the preparation steps are less.

The invention belongs to the technical field of biology, and particularly relates to polypeptide for promoting proliferation of mesenchymal stem cells and application of the polypeptide. The amino acid sequence of the polypeptide for promoting proliferation of the mesenchymal stem cells is shown as SEQ ID NO: 1. The active polypeptide for promoting proliferation of the umbilical cord mesenchymal stem cells is obtained by adopting a solid-phase synthesis method. Umbilical cord mesenchymal stem cells obtained by culturing the polypeptide have good adherence and multiplication capacities. In addition, the polypeptide can promote Nrf2 gene expression, so that proliferation of the umbilical cord mesenchymal stem cells is effectively promoted.

The invention relates to a molecular tag DMDPM compound, a preparation method thereof and application of the molecular tag DMDPM compound in assisting homogeneous synthesis of heptapeptide H6K, and belongs to the technical field of organic synthesis. The molecular tag DMDPM compound is 2, 4-dimethoxy-4 '-diphenylphosphinyl oxydiphenyl alcohol, and the molecular tag DMDPM compound is 2, 4-dimethoxy-4'-diphenylphosphinyl The method has the advantages of a liquid-phase synthesis method and a solid-phase synthesis method, H6K can be simply, quickly, economically and efficiently synthesized and prepared, and a 2, 4-dimethoxy-4 '-diphenylphosphinyloxy diphenyl alcohol small-molecule auxiliary group (also called as a carrier) can be recycled and directly reused, so that raw material waste is reduced, waste pollution is reduced, the cost is saved, and environmental protection is facilitated.

The invention discloses a synthesis method of an insulin analogue, which comprises the following steps of: firstly, obtaining A-chain peptide resin by using a solid-phase synthesis method, constructing a disulfide bond between A6 and A11 on a solid phase, and cracking the A-chain peptide resin by using a cracking solution containing a sulfydryl activator to obtain a peptide chain with an activated sulfydryl group and a protected sulfydryl group; then a solid-phase synthesis method is used for obtaining B-chain peptide resin, Lys side chain protecting groups are removed on a solid phase in a fixed-point mode, side chain fatty acid modification is completed, and a peptide chain with an exposed sulfydryl group and a protected sulfydryl group is obtained after cracking is conducted through a cracking solution; and mixing the products in a solution according to a certain proportion to form a first pair of intermolecular disulfide bonds, and constructing and purifying the last pair of disulfide bonds to obtain the insulin analogue. The method disclosed by the invention has the advantages of convenience in synthesis, low cost, simple process and the like, can be used for research on amino acid mutation of insulin compounds, and has important practical significance on development of insulin drugs.

The present application relates to the technical field of dielectric ceramic powder preparation, and particularly relates to a multilayer ceramic capacitor, a high-activity nano-barium titanate powder for the multilayer ceramic capacitor and a preparation method of the high-activity nano-barium titanate powder, the method comprising the following steps: (1) reacting a soluble barium salt with a precipitator to obtain barium carbonate precursor particles with high specific surface area; (2) uniformly coating nano-titanium dioxide particles on the surface of the barium carbonate precursor particles by using a supercritical fluid flash technology to form a composite precursor; and (3) performing a solid-phase synthesis reaction on the composite precursor and sintering to obtain nano-barium titanate powder. The present application, through the synergistic effect of the two means of "high-activity precursor preparation" and "nano-level uniform coating", prepares a composite precursor with extremely high specific surface area, surface energy and micro-uniformity, effectively reduces the heat sintering temperature, suppresses abnormal grain growth and lattice distortion, and significantly improves the tetragonality of the nano-barium titanate powder.

The invention discloses a continuous flow automatic polypeptide solid phase synthesis device which comprises a synthesis unit, a liquid storage unit, a waste output unit, a product bottle and a control unit, and the synthesis unit comprises a microchannel reactor, a washer, a circulating pump, a draw-off pump, a check valve and a product delivery pump; the liquid storage unit is connected with the draw-off pump, the draw-off pump is connected with the micro-channel reactor, the check valve is installed at the input end of the micro-channel reactor, the micro-channel reactor is connected with the washer, the waste output end of the washer is connected with the waste output unit, and the product output end of the washer is connected with the circulating pump and the product conveying pump. The circulating pump is connected to the micro-channel reactor, and the product conveying pump in the last synthesis unit is connected with the product bottle; and the control unit is connected with the circulating pump, the draw-off pump, the check valve, the product conveying pump and the waste output unit. The invention further discloses a continuous flow automatic polypeptide solid-phase synthesis method, and automatic polypeptide production is achieved.

The invention provides semeglutide, which is synthesized by adopting the following method, and the specific steps are as follows: 1) segmenting the main chain of semeglutide into three polypeptide fragments: 7-14 sites, 15-22 sites and 23-37 sites; (2) respectively preparing the 7-14-site fragments, the 15-22-site fragments and the 23-37-site fragments through solid-phase synthesis; 3) connecting the 7-14-site fragment with the 15-22-site fragment to form a 7-22-site fragment, and activating the C end of the fragment into active ester; (4) selectively removing an Alloc protecting group of Lys26 in the 23-37-site fragment, and then carrying out fatty acid modification to obtain a modified 23-37-site fragment; 5) in a liquid phase system, coupling the activated 7-22-site fragment and the modified 23-37-site fragment according to a molar ratio of 1: (0.6-1.4) to form a complete polypeptide chain; and 6) removing the protecting group and purifying to obtain a semaglutide finished product. The method provided by the invention can effectively realize high-purity, high-yield and low-cost synthesis of the semeglutide bulk drug.

The invention provides a synthesis method of tilpotide, which comprises the following steps: dividing a target peptide chain into six fragments, and adopting bis (4-C18-C28 alkoxy phenyl) methylamine, 2, 4-bis (18-C28 alkoxy)-benzyl alcohol and NH2-Asp (OTAG)-OR1 as hydrophobic label carriers to assist synthesis. A side chain carboxyl group of aspartic acid is innovatively used as an anchoring position of a hydrophobic label, a new fragment connection route is designed, a full-protection tilpotide conjugate is synthesized through a multi-label synergistic effect, and finally a protecting group and a label are removed by using a TFA lysate. Compared with a solid-phase synthesis method, the method is carried out in a homogeneous reaction, the dosage of amino acid and the condensing agent is reduced to 1-1.2 times from 2-3 times, and the cost is remarkably reduced. Compared with an existing hydrophobic labeling method, the method has the advantages that multiple labels can be introduced to serve as protecting groups, the yield and purity of synthesis of medium-chain and long-chain polypeptides are improved, meanwhile, the problem of hydrophobicity attenuation caused by peptide chain extension is solved, and the green chemical process requirement is met.

The invention discloses a polypeptide with DPP-IV (dipeptidyl peptidase-IV) inhibitory activity and application of the polypeptide. Pure peptides APFP and MPFP are obtained through a solid-phase synthesis method, the DPP-IV inhibition IC50 values of the pure peptides APFP and MPFP are measured to be 153.08 mu M and 296.50 mu M respectively, and the DPP-IV inhibition activity of the pure peptides APFP and MPFP is higher than that of partial fragments in the sequences of the pure peptides APFP and MPFP. The peptide fragments APFP and MPFP disclosed by the invention have relatively strong DPP-IV inhibitory activity, can be used for preparing hypoglycemic drugs or foods, and have wide application prospects in industrial application.

The invention relates to a method for semi-solid-phase synthesis of a polycyclic compound and an intermediate, a long chain is synthesized through solid phase, then two-step ring closing is performed to form a key intermediate, and simple derivation is performed on the basis of the key intermediate to obtain a PCSK9 antagonist compound. According to the invention, starting materials for solid-phase synthesis are selected, steric hindrance is effectively avoided, and solid-phase reaction and subsequent liquid-phase correlation cyclization can be smoothly carried out, so that the yield is improved, and the cost is reduced.

The invention relates to a ligand-induced room-temperature ultrathin magnetic nanosheet synthesis preparation method, which comprises: mixing a metal-ligand solution and an anion-ligand solution, and carrying out a heating reaction to obtain a ligand-induced room-temperature ultrathin magnetic nanosheet, wherein the metal-ligand solution comprises a Cu source, a Cr source and a first ligand; the anion-ligand solution comprises an anion X source and a second ligand; x is Se or Te; the first ligand is selected from one or two of oleylamine or oleyl alcohol; the second ligand is selected from one of oleylamine or tri-n-octylphosphine. Compared with the prior art, the method has the advantages that specific crystallographic orientation is stabilized by adjusting the adsorption capacity of ligands and surface ions in an organic liquid phase synthesis mode, anisotropic growth is guided, and the problems that in the prior art, room-temperature ultrathin nanosheet preparation excessively depends on substrate growth, and the steps are tedious are solved.

The invention belongs to the field of ceramic material synthesis, and discloses artificially synthesized jadeite and a liquid-phase synthesis method thereof. Natural low-quality jadeite is crushed by a crusher, magnetic black substances in the jadeite are removed through magnetic separation, purified powder is obtained after mixed acid pickling, and then the powder is subjected to high-temperature and high-pressure polymerization reaction to synthesize the artificial jadeite. The artificially synthesized jadeite prepared by adopting a liquid-phase high-temperature and high-pressure synthesis method has excellent density, gemstone characteristics and spectroscopic characteristics are basically consistent with those of natural jadeite, and the crystallinity is gt; 99%.

The invention discloses an oligonucleotide synthesis process of a sulfo-PMO structure. In the oligonucleotide synthesis process of the sulfo-PMO structure, the molecular structural formula of sulfo-PMO is shown in the specification. According to the invention, the molecular structure of thio-PMO is specifically limited, and the synthesis of nucleotide phosphate amide and (thio) phosphoric acid amide in the solid-phase synthesis oligonucleotide is carried out along the direction from 5'to 3 ', that is, in each cycle period, the O5'or O6' position of the nucleotide phosphate amide and (thio) phosphoric acid amide monomer is firstly subjected to coupling reaction, and then the protecting group is removed at the O3 'or N3' position, so that the oligonucleotide phosphate amide and (thio) phosphoric acid amide are obtained. And releasing active hydroxyl or amino / amido to enter the next cycle. The protecting group adopted by the sulfo-PMO molecule is consistent with the protecting groups of other nucleotides, so that the conversion rate of each step of coupling reaction can be conveniently detected on line.

The invention belongs to the technical field of luminescent materials. The invention discloses a CaF2-CaZnOS heterojunction stress luminescent material and a preparation method of the CaF2-CaZnOS heterojunction stress luminescent material. The chemical general formula of the heterojunction stress luminescent material disclosed by the invention is xCaF2-(10-x) CaZnOS: y% M, the used CaF2 and CaZnOS can realize the doping of transition metal Mn and various lanthanide series metals to realize stress luminescence, and realize the conversion under a force-induced spectrum in a heterojunction system, the CaF2 belongs to fluoride and can be partially used as a fluxing agent in the reaction process, the binding force of fluorine ions is strong, and the doping of fluorine can improve the stability of the material, so that the material can be widely applied to the field of luminescent materials. And the prepared stress luminescent material can be used for preparing a transparent substrate, and the application range is wider. According to the invention, a high-temperature solid-phase method is adopted for synthesis, the preparation process is simple, the cost is low, the composite heterojunction stress luminescent material with excellent luminescent characteristic is synthesized, the stress luminescence is visible under the condition of natural light, and the application potential is greatly enhanced.

The invention discloses a long-afterglow self-luminous material based on multi-element rare earth synergistic sensitization and a preparation method thereof. SrAlO is used as a matrix, trap level distribution is optimized through ternary rare earth synergistic doping according to the molar ratio of Eu to Dy to Nd being 1: (0.4-0.6): (0.2-0.4), and a ZnO nanorod array is grown on the surface of a light-emitting core in an in-situ epitaxial mode to improve the light extraction efficiency; and a hydrophobic modified SiO core-shell coating layer with an ordered mesoporous channel is combined, and oxygen diffusion is promoted by utilizing a nanopore channel so as to accelerate trap regeneration and synchronously inhibit non-radiative recombination. The afterglow time of the material is not less than 8 hours, and the afterglow retention rate after aging at 60 DEG C is not less than 80%. A solid-phase synthesis process and red mud / fly ash industrial solid waste raw materials are adopted, and the carbon emission intensity is smaller than or equal to 6 kgCO / kg. The material can be widely applied to the fields of green traffic infrastructures such as expressways and tunnels.

The present invention relates to an active oligopeptide RYIVPL, its preparation method and application. The active oligopeptide is RYIVPL, and its amino acid sequence is: Arg-Tyr-Ile-Val-Pro-Leu, which has the remarkable function of stimulating intestinal endocrine cells to secrete cholecystokinin (CCK). Compared with the prior art, the oligopeptide of the present invention can be artificially synthesized by a chemical solid-phase synthesis method, or can be obtained by enzymatic hydrolysis of wheat protein followed by separation and purification. The oligopeptide of the present invention has the characteristics of being safe, non-toxic and having no side effects, not being easily enzymolyzed by gastrointestinal digestive enzymes, and being easily absorbed, and is suitable as a functional component for developing drugs with the functions of delaying gastric emptying, promoting satiety and weight loss, and has great application value and broad prospects in the fields of medicine and the like.

The application relates to a synthesis method of an anti-freezing glycopeptide polypeptide and belongs to the technical field of polypeptide drug synthesis. The method comprises the following steps: 2-CL-Resin is used as a carrier resin, under the condition of adding an activating agent, the carrier resin and alanine are coupled to obtain Fmoc-Ala-2-CL-Resin; according to the amino acid sequence of the anti-freezing glycopeptide, other amino acids are sequentially coupled through a solid-phase synthesis method; after a protecting group is removed and the carrier resin is cleaved, the anti-freezing glycopeptide crude peptide is obtained; and after purification, salt conversion and freeze-drying, the anti-freezing glycopeptide polypeptide is obtained. The method has the advantages of short synthesis period, low cost, easy post-treatment, few by-products, high product yield, facilitation of large-scale production of the anti-freezing glycopeptide, and considerable economic applicative value and wide application prospect.

The invention discloses a low-temperature solid-phase synthesis cobalt blue pigment preparation method, which comprises: (1) placing a cobalt source, an aluminum source and an inert template dispersant in a planetary ball mill, carrying out ball milling, and drying to obtain nanometer composite precursor powder; (2) adding a mixture of a lithium source and a boron source into the nano composite precursor obtained in the step (1), putting the mixture into a mortar, and mechanically mixing to obtain a mixed material; and (3) putting the mixed material obtained in the step (2) into a muffle furnace, melting and calcining, cooling to room temperature along with the furnace, grinding, washing with hot water, and drying to obtain cobalt blue pigment powder. According to the method, the synthesis temperature is low, particle coarsening and sintering caused by high temperature are avoided, the energy consumption is low, the process is green, and the obtained cobalt blue pigment is pure in chromaticity, large in specific surface area and excellent in thermal stability.

A dual-modal information storage and anti-counterfeiting material, and its preparation method are provided. The dual-modal information storage and anti-counterfeiting material uses cadmium sulfide quantum dots (CdS QDs) as information storage material, and uses the controllable photocorrosion of CdS QDs to achieve dual-modal optical information storage and anti-counterfeiting applications. Firstly, the type of ligands and modification degree of CdS QDs are precisely controlled during the aqueous phase synthesise process, so as to effectively control the photocorrosion phenomenon under UV light irradiation. Subsequently, the CdS QDs are loaded in the hydrogel network, and they are also loaded on the substrates such as cloth and paper by spray coating, dip coating or 3D printing, and the information is stored by digital light patterning. Different from the photochromic function of traditional anti-counterfeiting material, the CdS QDs shows dual-modal patterning characteristics in a wide wavelength range.

The invention discloses a low-temperature plasma modified efficient hydrogen evolution catalyst. The method comprises the following steps: preparing a nano core-shell structure catalyst with uniform size through liquid-phase synthesis and layer-by-layer self-assembly, and introducing vacancies, defects and other unsaturated active sites on the surface of the nano core-shell structure catalyst; and then nitrogen and the like are used as a reaction atmosphere of a plasma chamber, and the surface of the catalyst is treated through a low-temperature plasma technology for catalyst performance regulation and control. The method has the advantages of simple process, low energy consumption, no need of adding extra chemical reagents, environmental friendliness and the like, and has a good application prospect. The preparation and regulation method of the electrocatalyst can be suitable for application of an electrocatalytic efficient hydrogen evolution catalyst. The material regulated and controlled by the plasma has higher current density and lower overpotential in hydrogen evolution reaction, and shows more excellent electrocatalytic activity and stability.

Provided is a method for producing a nickel powder with which it is possible to suppress the generation of linked particles in a liquid-phase synthesis method without hindering the reduction reaction of a nickel salt. A method for producing a nickel powder, the method including a step for starting a nickel precipitation reaction in a reaction solution in which a nickel salt, a metal having a lower ionization tendency than nickel or a salt thereof, a reducing agent, an alkali metal hydroxide, a sulfonium salt, and water are mixed, the sulfonium salt being used in an amount of 100 mol% or more relative to the nickel in the reaction solution.

The invention relates to the technical field of biological medicine, in particular to an improved preparation method of a GalNAc compound containing a ribose ring. Compared with an existing traditional synthesis route, the method has the advantages that the total yield of the whole reaction is remarkably increased, impurities are reduced, the purification mode is simplified, the cost is reduced, the method is environment-friendly and suitable for industrial production, and the obtained solid-phase carrier with high loading capacity is beneficial to amplified production of downstream oligonucleotide solid-phase synthesis.

A preparation method for semaglutide. The method comprises: producing a semaglutide resin by means of a solid-phase synthesis, producing crude semaglutide by cleavage and deprotection, producing refined semaglutide by purification and freeze-drying, comprising the solid-phase synthesis of a semaglutide 1-6 peptide fragment resin, which is cleaved and purified to serve as a first peptide fragment; and synthesizing a lysine having a sidechain group at locus 20 of semaglutide to serve as a second peptide fragment. In the method, prepared is a semaglutide loci 1-6 fully protected peptide fragment, which serves as a key starting material applied in the solid-phase synthesis of semaglutide, thus reducing the generation of D-His, D-Glu, D-Thr, D-Phe racemic impurities and +Gly impurities, reducing the difficulty of coarse product purification, increasing the purity and yield of semaglutide, reducing synthesis costs, and favoring industrialized large-scale production.

The present invention relates to the field of pharmaceutical technology, and discloses an anti-coronavirus polypeptide, a pharmaceutical composition and their applications. The anti-coronavirus polypeptide is based on the template EK1: SLDQINVTFLDLEYEMKKLEEAIKKLEESYIDLKEL-NH2 amino acid sequence. Through solid-phase synthesis, stapling and alanine modification are carried out on it, and the amino acids at specific positions are replaced with S5 and alanine. It is proved in the antiviral activity test that this kind of polypeptide molecule has anti-SARS-CoV-2 activity.

The present invention provides a use of a dipeptide fragment in solid-phase synthesis of a polypeptide compound, and a dipeptide fragment-based solid-phase synthesis method for a polypeptide compound. The dipeptide fragment is selected from the following structures: Gly-Gly, Ile-Aib, Tyr-Aib, Thr-αMePhe and Glu-Gly.