747results about How to "Short synthesis cycle" patented technology

The invention relates the field of medical synthesis and discloses a method for synthesizing liraglutide. The method includes: firstly synthesizing five polypeptide fragments of amino acid from first to fourth, amino acid from fifth to tenth, amino acid from eleventh to sixteenth, amino acid from seventeenth to twenty-fourth, and amino acid from twenty-fifth to thirty first according to amino acid sequence of the liraglutide main chain from N end to C end, and coupling the five polypeptide fragments to synthesize the liraglutide. Synthesizing of the five fragments can be performed simultaneously, synthesizing cycle is shortened greatly, total yield of the liraglutide can be increased, and accordingly the method is better than existing synthesizing methods.

The invention discloses a solid-phase synthesis method for liraglutide. The solid-phase synthesis method for liraglutide comprises the following steps: 1) firstly synthesizing first to tenth amino acid segments 3, eleventh to nineteenth amino acid segments 2, and twentieth to thirty-first amino acid segments 1, wherein the twentieth lysine adopts Fmoc-Lys(Mtt)-OH, and the first histidine adopts Boc-His(Trt)-OH; 2) synthesizing pal-Glu(OH)-Otbu by adopting a liquid phase synthesis method; 3) selectively removing the Mtt protecting group on the twentieth lysine by use of 5% TFA (Trifluoroacetic Acid), connecting pal-Glu(OH)-Otbu with the side chain of the twentieth lysine to obtain a segment 4; 4) sequentially connecting the segments 2, the segments 3 and the segments 4 to obtain peptide resin completely protected by liraglutide; 5) cracking, purifying, and lyophilizing to obtain the liraglutide product.

The invention discloses a metal-organic framework (MOF) material for permeating and separating gases and a preparation method thereof. Specifically, an MOF film disclosed by the invention is provided with a functional group, which contributes to nucleating on a substrate, increase the nucleating density on the substrate and contributes to the growth of a dense film; and the functional group can coact with certain specific gases, so that selective permeation of gases is facilitated. Due to the adoption of a film preparation method disclosed by the invention, the growing process of the film is simplified, the structure and shape of the film are optimized simultaneously, and film permeating and separating performance is enhanced. The MOF film prepared with the method has the advantages of high permeation amount, high separating coefficient, low energy consumption and avoidance of secondary pollution, and is particularly suitable for permeating and separating gases such as H2, CO2, CH4 and the like.

The invention discloses a complete solid-phase synthesis method for liraglutide. 2-Cl-TrtResin is enabled to serve as a solid-phase carrier. DIC/HOBt is enabled to serve as a condensation agent. After processing of microwave reaction technology, reaction time is shortened, and condensation efficiency is improved. According to side chain modification, novel ivDde side chain protected lysine is adopted and side chain modification synthesis is carried out. During the process, 20% piperidine is adopted to get rid of Fmoc protection until linear chain polypeptide synthesis is finished. Then, after hydrazine hydrate is adopted to get rid of ivDde protection, a side chain modification reaction is carried out. Obtained liraglutide with complete protection on the solid phase carrier is processed by trifluoroacetic acid, and crude liraglutide is obtained. After purification and freeze-drying by a C18 column, pure liraglutide is obtained. After strong negative ion salt conversion and free-drying, acetic acid liraglutide acetate is obtained. The complete solid-phase synthesis method for the liraglutide is simple in operation, short in synthesis cycle, low in production cost, few in accessory substance, high in product yield and beneficial for mass production.

The invention belongs to the pharmacochemistry technical field, and discloses a method for preparing polypeptide used for treating osteoporosis, concretely relates to a teriparatide preparation method. The preparation method is characterized by comprising the following steps: preparing each peptide resin fragment for forming teriparatide, gradually coupling each peptide resin fragment to teriparatide on a solid phase, then pyrolysizing to obtain the teriparatide crude product, and purifying to obtain the product teriparatide. Compared with the prior art, the preparation method has the advantages of simple operation, short synthesis cycle, low cost, less environmental pollution and high yield of teriparatide, and the total yield is 30%. The method of the invention is suitable for large-scale industrial production of teriparatide, and the prepared teriparatide has the advantages of high purity and less by-products, and has considerable economical and practical value as well as wide application prospect.

The invention discloses a method for synthesizing liraglutide. The method comprises the following steps of: 1, selecting Fmoc-Gly-Wang resin and N terminal Fmoc protected and side chain protected amino acid as raw materials, wherein lysine on a 26th site adopts Fmoc-Lys(Mtt)-OH or Fmoc-Lys(Mmt)-OH, histidine on an N terminal adopts Boc-His(Trt)-OH or Boc-His(Boc)-OH; 2, selectively removing a Mtt or Mmt protecting group on the lysine by adopting 1 percent TFA (Trifluoroacetic Acid); 3, sequentially coupling one g-glutamic acid and palmitic acid on a side chain; and 4, cutting resin by the TFA to obtain a crude product of the liraglutide, and carrying out preparative liquid chromatography purification and lyophilization to obtain a pure product of the liraglutide. The method for synthesizing the liraglutide is simple in steps, saves time and labor, is less in difficult sequences in a coupling process, simple and easy to operate during side chain de-protection, less in byproducts and high in yield, and is suitable for industrialized production.

The invention provides a preparation method and use of a Bi2O3/Bi2O4 phase heterojunction photocatalyst. The preparation method comprises the following steps: firstly, mixing 2.8 g of bismuth salt with 0-1.87 g of alkali uniformly to prepare a paste; then, placing a mixture into a muffle furnace and calcining at 100-450 DEG C for 0.5-4.0 h; washing a calcined substance with deionized water; and drying at 60 DEG C to obtain earthy yellow to reddish brown solids which are the Bi2O3/Bi2O4 heterojunction photocatalyst. The Bi2O3/Bi2O4 phase heterojunction photocatalyst prepared in the invention isused for degrading organic pollutants in water, and has higher visible light catalyzing activity than a commercial Bi2O3 photocatalyst.

The invention discloses a method for synthesizing highly-pure bendamustine hydrochloride, which comprises the following steps: taking [1-methy-2(4'-ethyl butyrate)-5-amino]-1H-benzimidazole as a raw material; and orderly reacting the [1-methy-2(4'-ethyl butyrate)-5-amino]-1H-benzimidazole with ethylene oxide and phosphorus oxychloride through the four steps of substitution, hydrolysis, salification and refinement so as to produce the bendamustine hydrochloride. The method in the invention is mild in condition, simple in operation, short in synthesis period and suitable for scaled-up industrial production; and the purity of the synthesized bendamustine hydrochloride is over 99.5 percent, while monomeric impurity is below 0.1 percent, which meet the quality standards of raw material medicament.

The invention provides a transition metal chalcogenide nanosheet material and a preparation method thereof, a battery anode material, a secondary battery and an application thereof, and belongs to thetechnical field of transition metal chalcogenides. The invention provides a preparation method of a transition metal chalcogenide nanosheet material, comprising the following steps: dissolving raw materials in an aqueous solution of soluble salt, removing moisture to obtain a solid, sintering the solid, and washing to obtain a transition metal chalcogenide nanosheet material, wherein the raw materials include a chalcogen precursor and a transition metal precursor. According to the preparation method, the soluble salt is used as a template, is inexpensive, is environmentally friendly and is easy to remove in post-treatment, and the obtained transition metal chalcogenide nanosheet material has a thinner sheet thickness. Compared with a traditional silica template method or a hydrothermal method, the preparation method of the invention greatly shortens the synthesis cycle, is simple and feasible, is controllable, has characteristics of high yield and simple experimental operation, and issuitable for large-scale production.

The invention relates to a solid electrolyte capable of lowering interface resistance on a metal lithium electrode, and a preparation method for the solid electrolyte. The preparation method comprises the steps of mixing lithium carbonate, lanthanum oxide and zirconium oxide, and uniformly grinding the mixture by a dry grinding method; then sintering the mixture in a muffle furnace, and grinding to obtain mother powder, and tabletting the mother powder; putting the tablet-shaped material into a crucible with a cover; then performing mother powder filling and sintering in the muffle furnace to obtain the compact ceramic sheet; and polishing the ceramic sheet until the surface of the ceramic sheet is smooth to obtain the solid electrolyte. Compared with the prior art, the electrolyte prepared by the method has the advantages of absence of impure phase on the surface, high relative density, low interface resistance on the metal lithium electrode, and the like.

The invention discloses a controllable method for preparing an orthogonal-phase stannous sulfide (SnS) two-dimensional monocrystalline nanosheet. The method includes the steps that a substrate is arranged on the downstream of a heating center of a horizontal tubular furnace and is 8-20 cm away from the heating center, SnS powder is placed in a high-temperature-resistant container, and the container is placed in the heating center of the horizontal tubular furnace; the tubular furnace is vaccumized, when the pressure intensity in the furnace is reduced to 0.1 Pa, inactive gas is injected into the furnace so that the pressure intensity in the tubular furnace can be 20-300 Torr again, and the flow speed of the gas is kept between 20 sccm to 200 sccm; the temperature of the heating center of the horizontal tubular furnace is raised to 600-800 DEG C, reaction time is 5-30 min, the substrate is taken out after the temperature in a cavity of the tubular furnace is naturally lowered to room temperature, and the stannous sulfide two-dimensional monocrystalline nanosheet grows on the surface of the substrate. The method is easy to operate, low in cost and high in controllability. Obtained SnS has the advantages of being large in size, good in uniformity and high in crystallinity, and the method has important research value and wide application prospects in the fields of field effect transistors, photoelectric detectors, photocatalytic hydrogen generation, lithium ion batteries and the like.

The invention discloses a molded metal-organic framework material and a molding method thereof. The molding method comprises the following steps: preparing a binder solution with a proper concentration to allow the binder solution to minimally block holes in a metal-organic framework material while maintaining good bonding performance; then uniformly mixing the binder solution with a suspension of the metal-organic framework material; placing a substrate membrane in the mixed solution obtained in the previous step to allow the surface of the substrate membrane to be uniformly adhered by a layer of the metal-organic framework material; and then soaking the substrate membrane uniformly adhered by the metal-organic framework material in an organic solvent to allow water molecules in the pore channels of the metal-organic framework material to be displaced out so as to reinforce the strength of the metal-organic framework material adhered on a substrate, wherein the molded metal-organic framework material with a large specific surface area and high mechanical strength is eventually obtained. Thus, the molding method provided by the invention overcomes the technical problems of complex molding process, a long molding period, severe conditions, high cost, severe loss of specific surface areas and the like in the prior art.

The invention discloses a solid phase synthesis preparation method of exenatide represented by a formula I, wherein a Fmoc-resin and a deprotection agent are mixed to obtain a deprotection resin, a Fmoc-amino acid and a deprotection resin are subjected to condensation to obtain a Fmoc-amino acid-resin, and Fmoc protection removal and condensation of the polypeptides on the Fmoc-amino acid and the resin are repeated to carry out condensation of the amino acid and the polypeptide on the resin according to a C terminal-to-N-terminal sequence to form a polypeptide resin. The method is characterized by comprising the following steps: (1) respectively forming polypeptide resin fragments represented by a formula II and a formula III; (2) cutting the fragment represented by the formula III to obtain a polypeptide fragment with complete side chain protection and represented by a formula IV; (3) conjugating the polypeptide fragment with complete side chain protection and represented by the formula IV to the polypeptide resin fragment represented by the formula II, and removing Fmoc to obtain a polypeptide resin represented by a formula V; (4) sequentially conjugating the remaining 10 Fmoc-amino acids, and removing Fmoc to obtain an exenatide-Rink Amide resin represented by a formula VI; and (5) separating the polypeptide and the resin on the polypeptide resin represented by the formula VI to obtain the exenatide represented by the formula I.

The invention discloses a preparing method of bicyclohexane monomer LCD in the monomer LCD preparing technical domain, which utilizes Grignard reaction to prepare the product with structural formula as graph I and synthetic feature route as graph II, wherein R1 and R2 is C2-C10; R3 is C1-C9 straight-chain alkyl; X is Cl or Br or I; A is C2H4 or cyclohexane; n is 0 or 1.