40 results about "Phase synthesis" patented technology

The application relates to the field of polypeptide medicine preparation, and particularly discloses a preparation method of bumenol peptide, which adopts a solid-liquid combination mode, liquid-phase synthesis of a tripeptide fragment Fmoc-Lys(Ac-Nle-Asp)-OMe, subsequent solid-phase synthesis of a cyclic heptapeptide methyl ester, cleavage, cyclization, deprotection and hydrolysis to obtain crude bumenol peptide. The cyclization site is alpha-COOH of Trp and alpha-NH2 of Lys, the reaction yield is high, and the cyclization problem between Lys and Asp in most current patents is solved. The process operation is simple, the deprotection reagent is conducive to environmental protection requirements. The crude product is easy to purify, the finished product has high yield and purity, and is suitable for industrial large-scale production.

The application provides a preparation method and application of a high near-infrared reflective red pigment. 1‑x RE x O5; wherein RE is at least one selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Y, Tm, Yb and Lu. The red pigment is obtained by doping with a rare earth element RE and using a high-temperature solid-phase synthesis method, so that the a* range of the red pigment is changed, and the redness and near-infrared reflectivity of the red pigment are improved.

A problem addressed by the present invention is to provide a method for efficiently producing a high-purity peptide compound at a high yield. It was discovered that an amino acid can be supported efficiently by a resin for solid-phase synthesis by bringing an amino acid solution including a specific solvent into contact with a resin for solid-phase synthesis swollen by a specific solvent, thereby solving the problem.

The invention provides an atomic precision metal cluster containing a multi-layer ligand spherical shell and a water phase synthesis method of the atomic precision metal cluster. The aqueous phase synthesis method comprises the following steps: performing first mixing on a metal precursor aqueous solution and a ligand aqueous solution, supplementing water to obtain an initial solution, and performing second mixing; then adding a reducing agent aqueous solution to obtain a reaction mixed solution; carrying out first stirring on the reaction mixed solution, concentrating, carrying out second stirring, and supplementing water; and repeating the operations of concentration, secondary stirring and water supplementation to obtain the atom precise metal cluster containing the multilayer ligand spherical shell. The multi-layer ligand spherical shell is adopted to protect the cluster, so that the cluster core can stably exist in an extremely long time without obvious change, and co-production, storage and utilization of related clusters are facilitated; and the metal clusters with uniform size and precise atoms can be directly obtained and have the same molecular weight, so that the post-treatment step can be simplified, and the feasibility of product amplification and application is enhanced.

The present application relates to the field of fluorescent material, and disclose a kind of samarium activated garnet-based red fluorescent powder, including Na, Gd, Sm, Ga, In and Ge, wherein, the amount-of-substance ratio of metal element is Na:Gd:Sm:Ga:In:Ge=1:2-2x:2x:2:1:2, x is the doping amount of samarium in inert rare earth site, 0.01≤x<0.10, the fluorescent powder proposed in the present application utilizes new garnet matrix constructed by sodium, gadolinium, gallium, indium, germanium, and has significant advantages compared to the traditional garnet isomorphic system constructed by containing aluminum, silicon, alkaline earth metal in preparation process.By using the new matrix, the reaction temperature of solid-phase synthesis fluorescent powder is greatly reduced, and no auxiliary solvent is needed, and it can be synthesized in one step.The preparation method of the present application does not require specific pressure and atmosphere requirements during the reaction process.This means that the preparation process is more flexible, and does not require high-pressure equipment or complex atmosphere control, simplifying the operation steps, improving the efficiency and feasibility of preparation.

This application discloses a method for manufacturing a CPG filter element, comprising: processing a CPG composite filter element, the CPG composite filter element comprising a core block and a CPG matrix integrally formed on the outside of the core block, the core block being resistant to the environment of the oligonucleotide synthesis process and at least partially exposed; and laser marking the exposed portion of the core block to form unique identification information for the CPG composite filter element. In subsequent oligonucleotide solid-phase synthesis operations, the CPG composite filter element of this application can be tracked based on the unique identification information on the core block, and traceability of the synthesis based on the CPG composite filter element can also be achieved. Furthermore, the embodiments of this application avoid the problems of easy detachment, corrosion, or blurring of markings due to traditional marking methods, leading to information loss, and also avoid the destruction of the integrity of the unique identification information during the high-temperature sintering process of the CPG filter element or the destruction of the pore structure of the CPG filter element by high-energy lasers.

The application provides an anti-coagulation protein Triabin containing a tyrosine sulfation modification and a semi-chemical synthesis method thereof. According to the distance, the Triabin is divided into fragment 1 and fragment 2 according to the closest cysteine to a sulfated tyrosine site, the sulfated tyrosine site is located in the fragment 1, and the sulfated tyrosine site is close to the C-terminal of the fragment 1; the polypeptide solid-phase synthesis technology is used to synthesize a fragment 1 polypeptide resin, and after cleavage, deprotection, extraction and purification, the fragment 1 with an amide C-terminal is obtained; the E. coli recombinant expression technology is used to obtain the fragment 2 with a hydrazine C-terminal; the thioester of the fragment 2 with the hydrazine C-terminal is converted, the natural chemical linking reaction and the neopentyl removal reaction are used to obtain a full-length linear protein, and the anti-coagulation protein Triabin containing the tyrosine sulfation modification is obtained through a refolding reaction. The anti-coagulation protein Triabin containing the tyrosine sulfation modification has stronger anti-coagulation activity than the wild-type Triabin.

The present invention relates to the fragment-based synthesis of peptides, in particular the peptide LL37. In specific the present invention relates to a method for fragmented solid phase synthesis of an LL37 peptide of SEQ ID NO: 1, or a variant thereof, comprising providing a first fragment of LL37, or a variant thereof, coupled to a first resin solid support by a cleavable linker, providing at least one further side chain protected fragment of LL37 coupled to a second resin solid support, wherein the fragment-resin linker is acid labile, cleaving the further side chain protected fragment(s) from the second solid support without deprotecting the side chains, and sequentially coupling the first and further fragments to produce a peptide of SEQ ID NO: 1, or a variant thereof.

The application discloses a kind of multiband adaptive phase shifter, belong to communication technical field, including input matching isolation module, routing switch S1, phase modulation module, discrete phase path module, topology reconstruction phase module, phase synthesis switch S7, compensation module and output matching isolation module, solve the technical problem that phase shifter is under the condition of multiband operation, consider phase regulation accuracy, amplitude consistency and adaptive path selection, different frequency band radio frequency signal is processed in the corresponding optimized phase modulation structure in the application, thereby avoid the problem of performance degradation of single phase shift structure under wideband condition, the amplitude attenuation and phase deviation introduced to different paths are corrected, improve the phase consistency and amplitude stability of output signal under the condition of multiband, can realize quick switching and high integration design, suitable for wideband, multiband and fast response radio frequency system.

The application discloses a caviar polypeptide composition with enhanced immune function, a preparation method, application and preparation, belongs to the technical field of bioactive polypeptides, and comprises at least one polypeptide with an amino acid sequence of RWFPGKPLFWRA, FWKPLRGALFPW or KWRFPGALPWFA and a molecular weight of 1400-1550 Da. The preparation method comprises caviar protein extraction, complex enzymolysis, ultrafiltration separation, chromatography purification and solid-phase synthesis. Animal experiments prove that the polypeptide can significantly enhance cell immunity, humoral immunity, monocyte-macrophage function and NK cell activity, the mechanism is related to TLR2 / TLR4 receptor activation and NF-κB / MAPK signal pathways, the safety is good, and the polypeptide is suitable for development into an immune-enhancing health food or medicine.

This invention belongs to the field of environmental protection and discloses a method for synthesizing metal-organic frameworks (MOFs) using a one-pot aqueous phase method. The method includes the following steps: mixing an amino- or aldehyde-containing pyrazolyl derivative, an aldehyde- or amino-containing linker, a copper salt, and pyruvate; adding an acidic solution of water; and then sonicating or stirring at room temperature to obtain a highly crystalline MOF. The amount of pyruvate used may be zero or not zero. When an amino-containing pyrazolyl derivative is selected as the raw material, an aldehyde-containing linker is selected; when an aldehyde-containing pyrazolyl derivative is selected as the raw material, an amino-containing linker is selected. The one-pot aqueous phase synthesis method provided by this invention eliminates the use of organic solvents, greatly reducing environmental impact. It also allows for large-scale synthesis with good reproducibility, a simple synthesis process, and strong operability, showing broad application prospects.

This invention provides a hypophosphite derivative, its preparation method, and a liquid-phase synthesis method for peptides using the hypophosphite derivative as a carrier, belonging to the fields of organic synthesis and peptide chemistry. In this invention, a hypophosphite derivative is prepared. The hypophosphite derivative provided in this application has advantages such as simple preparation method, low-cost raw materials, and easily adjustable structure. The peptide liquid-phase synthesis method using the hypophosphite derivative as a carrier can efficiently synthesize peptides and improve the solubility of intermediates in the preparation process of peptides (especially hydrophobic peptides), avoiding aggregation or precipitation, and has practical application value for peptide chemical synthesis.

The application discloses a homogeneous phase synthesis method of copper-based micro-nano materials with controllable phase and morphology, which comprises the following steps: (1) dissolving soluble copper salt in a mixed solvent of ethylene glycol and ethylenediamine, and stirring to obtain a clear homogeneous phase solution; (2) adjusting the adding amount of deionized water in the reaction system to determine the phase of the product as copper or cuprous oxide or a composite material of both; (3) under the determined phase system, adjusting the adding amount of ethylene glycol in the reaction system to control the micro-morphology and exposed crystal face of the product; and (4) performing low-temperature solvothermal reaction under sealed conditions, and obtaining the target product through centrifugation, washing and drying after the reaction is completed. The method has the advantages of simple process, no need of solid precursors and high-temperature calcination in the whole process, mild reaction condition, high product purity, good repeatability and the like, and effectively solves the problem that the prior art is difficult to simultaneously and accurately control the crystal structure and micro-morphology of copper-based materials in the same system.

This invention discloses a chiral CuO / HgS heterojunction catalyst, its preparation method, and its application, belonging to the field of inorganic chiral materials technology. The chiral CuO / HgS heterojunction includes D-CuO / D-HgS heterojunction, L-CuO / L-HgS heterojunction, D-CuO / L-HgS heterojunction, and L-CuO / D-HgS heterojunction. Its preparation method includes: (1) preparing chiral CuO powder using a liquid-phase synthesis method with chiral cysteine ​​and CuCl2; (2) obtaining chiral HgS crystal nuclei by reacting Hg(NO3)2 solution with chiral penicillamine and thioacetamide, and dispersing them in water to obtain chiral HgS seed colloids; (3) synthesizing chiral CuO / HgS heterojunctions using a seed-mediated epitaxial growth method. Using the prepared chiral material for photocatalytic CO2 reduction can yield high-value-added C2 and C3 products, achieving efficient energy utilization.

Disclosed herein are novel methods for the preparation and purification of oligonucleotides, such as those for use in therapy. In particular, the novel methods disclosed herein involve a three-reaction cycle of solid-phase synthesis and eliminate the need for chromatography purification.

The application discloses a preparation method of deuterium or tritium labeled oligonucleotide, which adopts a combination of solid-phase synthesis and liquid-phase synthesis for the first time, and successfully prepares 5' end deuterium or tritium labeled oligonucleotide. The application can not only precisely control the labeling site of deuterium or tritium, avoid non-specific labeling, but also significantly improve the specific activity of tritium labeled oligonucleotide, and provides a new technology for the synthesis of labeled oligonucleotide.

The present application relates to the technical field of bioengineering, in particular to a collagen peptoid and a preparation method and application thereof. The present application provides a method different from conventional solid-phase synthesis of collagen peptoids. The preparation method of the collagen peptoid provided only needs two-step reactions of polymerization (random polycondensation) and hydrogenation catalysis, and the reactions are carried out in a homogeneous solution, so that the preparation method is simple and suitable for large-scale industrialized preparation. Moreover, the structure of the collagen peptoid provided can be flexibly changed according to needs on the basis of different monomer proportions, and the target peptoid can be quickly prepared.

The application discloses a synthesis method of phosphorodiamidate morpholino oligonucleotide, belongs to the technical field of solid-phase synthesis of phosphorodiamidate morpholino oligonucleotide, and specifically relates to the following steps: adding 9-fluorenylmethyloxycarbonyl-piperazine-succinic acid into Wang resin to mix and react to synthesize 9-fluorenylmethyloxycarbonyl-piperazine-succinic acid-Wang resin, then adding phosphoramidite monomers to perform coupling reaction after deprotection treatment, performing cap treatment after the coupling is completed, then repeatedly performing deprotection treatment, coupling reaction and cap treatment until the coupling of all phosphoramidite monomers is completed, then removing the protecting group of the last phosphoramidite monomer, and then performing cleavage treatment and deprotection treatment of a base protecting group to obtain a phosphorodiamidate morpholino oligonucleotide (PMO) reaction solution. The application provides a synthesis method of phosphorodiamidate morpholino oligonucleotide with high coupling efficiency, low impurity level, high yield and high purity.

This invention provides a liquid-phase synthesis apparatus, comprising: a liquid-phase synthesis vessel, wherein the liquid-phase synthesis vessel includes a synthesis vessel body, an upper baffle plate, a lower baffle plate, and an external heat exchanger. Compared with the prior art, this invention has the following beneficial effects: by adding a liquid-phase synthesis vessel and a vessel cover assembly, the vessel cover assembly is sealed and installed above the synthesis vessel body. The upper and lower stirring blades are driven by the stirring shaft to stir, and a convection structure is achieved. The liquid impacts the upper and lower baffle plates during stirring, forming turbulence, which makes the mixture form a complex flow structure. In the constant temperature control, the built-in upper and lower baffle plates and the external heat exchanger improve the temperature control effect, thereby improving the liquid-phase synthesis effect. By adding the synthesis vessel assembly, the feed conduit guides the raw material to the feed distribution pipe, and the raw material falls into different areas through the discharge hole during spiral conveying, thereby further improving the liquid-phase synthesis effect.

A novel production method of a compound having a structure in which a saccharide skeleton is introduced into an amino acid derivative. When producing a glycoprotein as the compound, solid-phase synthesis of a peptide is unnecessary, formation of a non-natural structure is unnecessary, and a production method with a low degree of limitation of applicable saccharides is provided. 【Solution means】A compound represented by the following formula (where R 1 is an acetylamino group or a hydroxyl group; R 2 , R 3 , R 4 and R 5 are an alkyl group, an aryl group or an aralkyl group; G 1 is a hydrogen atom, a methyl group, or a group represented by the general formula -CH2-OX 3 ; X 1 , X 2 and X 3 are a hydrogen atom, a monovalent group having a structure in which the anomeric hydroxyl group in a saccharide is removed, etc.). TIFF2026084686000104.tif46170

This invention belongs to the field of solid-phase synthesis technology. A method for preparing aflatoxin lysine adduct based on solid-phase synthesis includes the following steps: (1) synthesis of an amino acid-supporting resin; (2) deprotection of the amino acid resin to obtain N-α-Boc-lysine resin; (3) cyclization to obtain N-ε-aflatoxin dialdehyde-N-α-Boc-lysine resin; (4) oxidation to obtain N-ε-aflatoxin-N-α-Boc-lysine resin; (5) cleavage and purification to obtain the aflatoxin lysine adduct. This invention provides an aflatoxin lysine adduct. This invention also provides a standard for the aflatoxin lysine adduct. This invention utilizes solid-phase synthesis technology to synthesize aflatoxin amino acid adducts on resins, especially the efficient synthesis of AFB1-Lys, providing reliable standards for clinical medical diagnosis and food testing. Particularly in the determination of serum albumin aflatoxin adducts, it greatly assists in the accurate monitoring of aflatoxin exposure levels.

The application relates to an azobenzene quencher unit, a preparation method thereof, a solid-phase synthesis carrier, a preparation method thereof, and a nucleic acid probe. The structural general formula of the azobenzene quencher unit is shown in the following formula: wherein R1, R2, R3, R4, R5, R6, R7, R8, R9, R10, R11, R12 and R13 are independently hydrogen, methyl, ethyl, propyl, isopropyl, phenyl, biphenyl, 2-furyl, 2-thienyl, methoxy, ethoxy, isopropoxy, nitro, nitroso or cyano, n=0-6, and m=2-12. The azobenzene quencher unit contains a polyfluorocarboxylic acid connecting structure. The azobenzene quencher unit is connected to the solid-phase synthesis carrier through the formation of an amide bond between the carboxylic acid of the polyfluorocarboxylic acid connecting structure and the amino group on the surface of the solid-phase synthesis carrier, and is used for synthesizing nucleic acids. The synthesis yield of 3' azobenzene quencher-labeled nucleic acids can be effectively improved.

This invention discloses a low-temperature solid-phase synthesis method for manganese tetroxide, belonging to the field of inorganic functional material preparation technology. The preparation method includes: preparing a targeted organic ammonium salt surface modifier; preparing a composite precursor by high-energy ball milling of a manganese source (γ-type MnOOH) and a rhombohedral MnCO3, a modifier, and a composite auxiliaries; obtaining a crude product through a low-temperature solid-phase reaction at 220-350℃ under a nitrogen or argon inert atmosphere; and obtaining the final product through fluidized bed desorption, air jet milling depolymerization, sieving, acid washing, and vacuum drying. To address the shortcomings of existing solid-phase synthesis methods, such as high energy consumption, easy generation of impurities, and product agglomeration, this invention proposes a synergistic regulation and low-temperature solid-phase synthesis technology. Through specific manganese source formulation and the synergistic effect of modifiers and auxiliaries, pure-phase synthesis at 220-350℃ is achieved, solving problems such as high-temperature dependence and impurity phase formation. The product has a regular crystal structure, high purity, and good dispersibility, making it suitable for high-end lithium-ion battery cathode materials and other applications. The process is energy-efficient and environmentally friendly.

This invention relates to the field of peptide drug preparation techniques, specifically disclosing a method for the hydrophobic tag-assisted liquid-phase synthesis of retatrutide. The retatrutide preparation method includes the following steps: synthesizing two hydrophobic tags, TAG1 and TAG2; dividing retatrutide into six fragments and linking each fragment to a TAG; wherein the C-terminal amino group of TAG2 can be directly retained after deprotection; the peptide fragments obtained during synthesis can be purified by acetonitrile slurrying; the main chain of retatrutide is obtained by end-to-end ligation, followed by the ligation of side chains to obtain fully protected retatrutide; finally, deprotection and removal of the hydrophobic tag are performed to obtain retatrutide. The preparation method of this invention uses readily available starting materials, and the reaction operations and separation / extraction processes in each step of the synthesis route are simple, the conditions are mild, the overall yield is high, and material costs are significantly reduced.

The present application relates to the field of eggshell membrane peptides, and provides an anti-aging eggshell membrane peptide, a solid-phase synthesis method and application thereof, an anti-aging eggshell membrane peptide composition and a preparation method thereof, wherein the anti-aging eggshell membrane peptide is a polypeptide with an amino acid sequence as shown in SEQ ID NO. 1. The amino acid sequence is LGPVGYPKLR, i.e. Leu-Gly-Pro-Val-Gly-Tyr-Pro-Lys-Leu-Arg. The present application screens an eggshell membrane peptide with good anti-aging effect from an eggshell membrane hydrolysate, and synthesizes a polypeptide with a corresponding amino acid sequence by using a solid-phase synthesis method, so that the industrialization of the anti-aging eggshell membrane peptide can be simply realized, and the eggshell membrane peptide can be applied to anti-aging products.

Provided is a method for preparing lutetium[177Lu]dotatate and a precursor compound thereof, comprising performing coupling reactions on Fmoc-Thr(tBu)-OH, Fmoc-Cys(Trt)-OH, Fmoc-Thr(tBu)-OH, Fmoc-Lys(Boc)-OH, Fmoc-D-Trp(Boc)-OH, Fmoc-Tyr(tBu)-OH, Fmoc-Cys(Trt)-OH, Fmoc-D-Phe-OH, and DOTA-(tBu)3-CO2H successively on a Wang resin by means of a solid-phase synthesis method to obtain DOTA-(tBu)3-D-Phe-Cys(Trt)-Tyr(tBu)-D-Trp(Boc)-Lys(Boc)-Thr(tBu)-Cys(Trt)-Thr(tBu)-Wang resin, performing an oxidation reaction to remove Trt protecting groups from two Cys residues and form a disulfide bond therebetween, thus achieving cyclization, and then performing a cleavage reaction to remove the Wang resin and protecting groups to obtain a lutetium[177Lu]dotatate precursor compound represented by formula I. The preparation method can significantly improve the purity of the prepared lutetium[177Lu]dotatate precursor compound, reduce the impurity content, improve the product yield, and simplify the subsequent purification process.

This invention belongs to the technical field of peptide liquid-phase synthesis carriers, and discloses a soluble liquid-phase carrier for peptide liquid-phase synthesis and its application. The structural formula of the soluble liquid-phase carrier for peptide liquid-phase synthesis is as follows, wherein: the group R is selected from H, methoxy, halogen, alkyl, aldehyde, and nitro groups, and the number is 1-3; the number of Linker-Tag groups is 1-3. When the soluble liquid-phase carrier of this invention is applied to peptide liquid-phase synthesis, it not only exhibits excellent performance in improving operational efficiency and facilitating reaction monitoring, but also has the advantages of economy and sustainable use. It can significantly improve the efficiency and controllability of the peptide liquid-phase synthesis process and has strong practicality.

The application discloses a liquid-phase synthesis method of cis-1-chloro-2,3,3-trifluoropropene and application thereof, and belongs to the technical field of organic synthesis. The method comprises the following steps: performing a dehydrofluorination reaction on 3-chloro-1,1,2,2-tetrafluoropropane in the presence of polyethylene glycol and an aqueous inorganic base solution to prepare cis-1-chloro-2,3,3-trifluoropropene; the molecular weight of the polyethylene glycol is 200-600 g / mol; and the polyethylene glycol can be hydroxyl-terminated polyethylene glycol or alkoxyl-terminated polyethylene glycol. The method realizes efficient synthesis of cis-1-chloro-2,3,3-trifluoropropene, is green, environment-friendly and efficient, has a short synthesis route, high conversion rate and high selectivity, the selectivity of cis-1-chloro-2,3,3-trifluoropropene is greater than or equal to 90%, and the yield of cis-1-chloro-2,3,3-trifluoropropene is greater than or equal to 80%.

This invention discloses an amphiphilic phenolic network nanosphere, its preparation method, and its applications. The nanospheres possess an intrinsically amphiphilic topology of a hydrophobic aromatic network core and a hydrophilic hydroxyl-rich shell, and are monodisperse spherical particles with dodecyltrimethylammonium bromide anchored on their surface. This invention also provides a one-step aqueous synthesis method, achieving precise size control through the introduction of phase separation and interface modifiers. The synergistic dispersion system formed by the nanospheres and sodium fatty alcohol polyoxyethylene ether sulfate is stably dispersed in a high-salt environment (>10,000 mg / L), with an oil-water interfacial tension as low as 1.03 mN / m, capable of reversing oil-wetted core surfaces to water-wetted surfaces (contact angle ≤70°). The nanospheres of this invention can spontaneously adsorb at the oil-water interface and self-assemble under the Marangoni effect to form a high-strength particle-reinforced interfacial film. This invention provides new materials and methods for efficient oil recovery in complex reservoirs.