22 results about "Tetramethylurea" patented technology

The invention discloses a preparation method and application of a compound with a cold sensing regulation effect, which comprises the following steps: dissolving tryptophan in methanol, adding concentrated sulfuric acid, esterifying the acid to protect carboxyl so as to obtain tryptophan methyl ester, dissolving the obtained tryptophan methyl ester and aromatic carboxylic acid substances in N, N-dimethylformamide, and reacting to obtain the compound with the cold sensing regulation effect. The method comprises the following steps: catalyzing 2-(7-azabenzotriazole)-N, N, N ', N'-tetramethylurea hexafluorophosphate and N, N-diisopropylethylamine, dissolving a catalyzed product in ethanol (98%), adding into a NaOH solution, stirring, carrying out rotary evaporation treatment, slowly dropwise adding a 0.5 mol / L hydrochloric acid solution, adjusting the pH value of a reaction system to 3-4, and finally obtaining the tryptophan derivative compound with the yield of 70%. The invention provides a potential medicine for improving the working ability and cold injury in the cold environment for people living and working in the cold environment, and is developed into a medicine for effectively improving neuropathic pain diseases in the cold environment.

The invention discloses a method for synthesizing dipeptide Fmoc-Leu-Aib-OH, and belongs to the field of polypeptide synthesis, the specific preparation method comprises the following steps: under the action of organic alkali and an activating reagent, Fmoc-Leu-OH and H-Aib-OH react to obtain the dipeptide Fmoc-Leu-Aib-OH; the activating reagent comprises at least one of N, N, N ', N'-tetramethyl chloroformamidine hexafluorophosphate, 2-(7-azabenzotriazole)-N, N, N ', N'-tetramethyl urea hexafluorophosphate and benzotriazole-1-yl-oxytripyrrolidinyl phosphorus hexafluorophosphate, and the organic base comprises at least one of N-methylimidazole, N, N-diisopropylethylamine and pyridine. The dipeptide Fmoc-Leu-Aib-OH prepared by the preparation method disclosed by the invention is high in yield, high in purity and high in raw material conversion rate.

The invention discloses a production method of a hexafluorophosphate product, the hexafluorophosphate product is 2-(inner-5-norbornene-2, 3-dicarboximide)-1, 1, 3, 3-tetramethylurea hexafluorophosphate, the first-step reaction of the invention comprises the following steps: preparing an intermediate from norbornene dianhydride as a raw material and a hydroxylamine compound under the action of organic alkali; in the second-step reaction, the intermediate and TCFH are subjected to a nucleophilic substitution reaction under the action of an alkaline metal catalyst to obtain a crude product, and the crude product is purified to obtain a target product; the synthesis route used in the invention is simple, special high temperature or high pressure is not needed in the reaction process, and the used catalyst is a conventional raw material which is low in price and easy to obtain; according to the method, the purity of the product can be increased to 99.8% or above, the total yield is stabilized to be 85% or above, in addition, the reaction route greatly reduces side reactions, and by-products in the product are few in variety and low in content.

The invention provides fluorescein and a purification and synthesis method thereof, and relates to the field of compound preparation. The method comprises the following steps: carrying out first mixing and first reaction on 4-(aminomethyl) benzoic acid, triethylamine, a first organic solvent and trifluoroacetate to obtain a first intermediate; performing second mixing on the first intermediate, a second organic solvent, triethylamine and 2-succinimido-1, 1, 3, 3-tetramethylurea tetrafluoroborate, and performing second reaction to obtain a second intermediate; and carrying out third mixing on the second intermediate, amino FAM, a third organic solvent and triethylamine, and carrying out third reaction to obtain fluorescein. The synthesis and purification method is efficient, and fluorescein can be rapidly obtained without column chromatography; chemical raw materials used in the synthesis method are simple and easy to obtain, the cost is low, reaction conditions are mild, amplified production is easy, the purification method is simple and convenient to operate, and the obtained intermediate is high in stability.

The invention belongs to the technical field of biochemistry, and relates to a ratio type probe compound, a preparation method thereof, a Cu (I) response photoacoustic probe composition and application. The preparation method of the ratiometric probe compound comprises the following steps: (1) reacting a compound (I), a compound (II), acetic acid and piperidine to obtain a compound (III); (2) reacting the compound (III) with trifluoroacetic acid to obtain a compound (IV); (3) carrying out a reaction on the compound (IV), the compound (V), 2-(7-azabenzotriazole)-N, N, N ', N'-tetramethylurea hexafluorophosphate and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride, so as to obtain a compound (VI); and (4) reacting the compound (VI), the compound (VII), acetic acid and piperidine to obtain the compound. The photoacoustic probe provided by the invention has excellent selectivity and high sensitivity.

The application belongs to the technical field of biochemistry, and relates to a ratio type probe compound, a preparation method thereof, a Cu(I) response photoacoustic probe composition and application. The preparation method of the ratio type probe compound comprises the following steps: (1) reacting compound (I), compound (II), acetic acid and piperidine to obtain compound (III); (2) reacting compound (III) and trifluoroacetic acid to obtain compound (IV); (3) reacting compound (IV), compound (V), 2-(7-azabenzotriazole)-N,N,N',N'-tetramethyluronium hexafluorophosphate and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride to obtain compound (VI); and (4) reacting compound (VI), compound (VII), acetic acid and piperidine to obtain the compound. The photoacoustic probe provided by the application has excellent selectivity and high sensitivity.

The invention discloses a fluorescent probe for detecting the viscosity of a cell membrane as well as a preparation method and application of the fluorescent probe, and belongs to the technical field of small molecule probes. The structural formula of the fluorescent probe is shown in the specification. The preparation method specifically comprises the following steps: (1) reacting 4-diethylaminoketonic acid and cyclohexanone in concentrated sulfuric acid, pouring into crushed ice, stirring, adding perchloric acid, stirring, standing and filtering; (2) dissolving 4-diethylaminobenzaldehyde in absolute ethyl alcohol, heating and refluxing, removing the solvent, and carrying out chromatography; and (3) dissolving benzotriazole-N, N, N ', N'-tetramethylurea hexafluorophosphate and N, N-diisopropylethylamine in N, N-dimethylformamide, stirring at normal temperature, adding a compound 43-(tetradecyl amino) propane-1-sulfonate, continuously stirring, removing the solvent, and carrying out chromatography to obtain the compound 43-(tetradecyl amino) propane-1-sulfonate. The fluorescent probe has excellent anchoring and imaging capabilities and viscosity-triggered near-infrared (NIR) fluorescence response characteristics, can be used for fluorescence imaging of cell membrane viscosity, and can also be used for viscosity imaging analysis of breast cancer mice.

The invention belongs to the technical field of magnesium ion batteries, and discloses a water-based magnesium ion battery electrolyte and a preparation method and application thereof, and the mixed electrolyte for the water-based magnesium ion battery is composed of magnesium salt, an organic solvent and deionized water; wherein the organic solvent is tetramethylurea (TMU), the tetramethylurea and the deionized water jointly form a mixed solvent of the mixed electrolyte, the volume percent of the tetramethylurea in the mixed solvent is 10%-50%, and the volume percent of the deionized water in the mixed solvent is 90%-50%; the magnesium salt is dissolved in the mixed solvent. The components of the electrolyte are improved, the TMU is taken as the mixed electrolyte of the cosolvent, and the volume fraction of the TMU is accurately regulated and controlled, so that the problem of short cycle life caused by narrow electrochemical stability window (ESW) and serious interface side reaction of the water-based magnesium ion battery is solved, and the electrolyte has the advantages of simplicity in preparation, environment friendliness and low cost, and is suitable for industrial production. A new way is provided for improving the energy density and the cycle life of the water-based magnesium ion battery.

This invention relates to a coating solution for composite lithium-ion battery separators, a composite lithium-ion battery separator, and a method for preparing the same. The coating solution for composite lithium-ion battery separators comprises: (A) poly(p-phenylene terephthalamide); (B) an organic solvent, which is at least one selected from hexamethylphosphoramide and tetramethylurea; (C) a co-solubilizing salt, which is at least one selected from lithium chloride and calcium chloride; and (D) an additive, which is at least one selected from ceramic powder and polymer binder. The coating solution for composite lithium-ion battery separators exhibits good stability. The composite lithium-ion battery separator possesses good air permeability, heat resistance, and good compatibility with the electrolyte, making it suitable for lithium-ion batteries. The preparation methods for both the coating solution and the composite lithium-ion battery separator are simple, convenient, and have low production costs.

The present invention provides a method for synthesizing 4-bromo-N-(2,6-dioxopiperidin-3-yl)-2-fluorobenzamide, which relates to the field of organic chemical synthesis technology and includes a one-step reaction. Specifically, it involves using 4-bromo-2-fluorobenzoic acid and 3-aminopiperidin-2,6-dione hydrochloride as raw materials, N,N-dimethylformamide as solvent, and adding triethylamine and 2-(7-azabenzotriazole)-N,N,N',N'-tetramethylurea hexafluorophosphate to obtain the target product 4-bromo-N-(2,6-dioxopiperidin-3-yl)-2-fluorobenzamide. The synthesis method of the present invention has a short process route, inexpensive and readily available raw materials and excipients, high reactivity, simple operation, easy control, and a high yield of the target product, which is convenient for industrial scale-up.

The present invention relates to the technical field of specific molecular targeted diagnostic reagents. Provided are a near-infrared fluorescent probe for active targeting detection of an epidermal growth factor receptor, and a preparation method therefor and the use thereof. The preparation method comprises: mixing N-(3-chloro-2-fluorophenyl)-7-methoxy-6-(piperidin-4-yloxy)quinazolin-4-amine and X in the presence of 2-(7-azabenzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate, a base and a polar solvent; adding the product dropwise to water; extracting the suspension with an organic solvent, followed by drying and concentration; removing the protecting group from the concentrate, followed by column chromatography to obtain an intermediate compound; and adding the intermediate compound to 2-(7-azabenzotriazol-1-yl)-N,N,N',N'-tetramethyluronium hexafluorophosphate, a base, Y and a polar solvent, followed by purification to obtain the near-infrared fluorescent probe. The prepared near-infrared fluorescent probe can achieve the effect of in-vivo diagnosis.

The invention discloses a lysosome targeted copper ion fluorescent probe with an AIE (aggregation-induced emission) effect, which is obtained by taking 7-(diphenylamino)-2-oxo-2H-benzopyran-3-carboxylic acid (I) and 8-aminoquinoline (II) as raw materials and reacting and synthesizing under the action of 2-(7-azabenzotriazole)-N, N, N ', N'-tetramethylurea hexafluorophosphate and triethylamine. The chemical structural formula of the fluorescent probe is shown as a formula (III), and the fluorescent probe has an AIE effect, has the advantages of high selectivity and high sensitivity on Cu < 2 + > recognition and the like, and can be used for effectively detecting Cu < 2 + > in an environmental water sample; besides, the probe has good biocompatibility, can be positioned in a lysosome, and is applied to real-time fluorescence imaging monitoring of Cu < 2 + > concentration change in an autophagy process caused by starvation or a chemical inducer in living cells and zebra fish bodies; the invention provides a copper ion detection tool with excellent performance, which has huge potential in the fields of environmental monitoring and life science research.

The invention discloses a method for improving the production capacity of II type full-length collagen of pichia pastoris. The method comprises the following steps: in a methanol-induced pichia pastoris fermentation production system, adding three stabilizers, namely dimethyl sulfoxide (DMSO), 4-phenylbutyric acid (4-PBA) and tetramethylurea (TMU), into a fermentation culture medium in a combined manner. According to the method, the yield of the complete recombinant human II type full-length collagen is remarkably improved, and compared with the sum of target protein yield improvement effects of independently using the three stabilizers, the combined use of the three stabilizers achieves a synergistic target protein yield improvement effect. The method also has the advantages of simple process, low cost, no need of gene modification and easiness in large-scale production.

The present invention provides a method for synthesizing 4-bromo-N-(2,6-dioxopiperidin-3-yl)-2-fluorobenzamide, which relates to the field of organic chemical synthesis technology and includes a one-step reaction. Specifically, it involves using 4-bromo-2-fluorobenzoic acid and 3-aminopiperidin-2,6-dione hydrochloride as raw materials, N,N-dimethylformamide as solvent, and adding triethylamine and 2-(7-azabenzotriazole)-N,N,N',N'-tetramethylurea hexafluorophosphate to obtain the target product 4-bromo-N-(2,6-dioxopiperidin-3-yl)-2-fluorobenzamide. The synthesis method of the present invention has a short process route, inexpensive and readily available raw materials and excipients, high reactivity, simple operation, easy control, and a high yield of the target product, which is convenient for industrial scale-up.

The invention discloses a method for in-situ labeling and synchronous promotion of extracellular vesicle secretion, and a preparation method of a glucose modified photosensitizer comprises the following steps: carrying out an amidation reaction on glucosamine, a photosensitizer, benzotriazole-N, N, N ', N'-tetramethylurea hexafluorophosphate, 4-(dimethylamino) pyridine and N, N-diisopropylethylamine in a solvent, cooling to room temperature, filtering, washing, and drying to obtain the glucose modified photosensitizer. According to the glucose-modified photosensitizer and the preparation method thereof disclosed by the invention, the glucose is modified by the photosensitizer to be loaded into the EV by utilizing the metabolic process of the glucose, so that the drug loading rate of a disease treatment drug can be improved while the integrity of an EV membrane is maintained; and negative side effects of physical or chemical intervention are avoided, so that the functional EV with higher purity is obtained.

The application discloses a preparation method of a bile acid-norfloxacin compound, which comprises the following steps: reacting bile acid and norfloxacin in the presence of 2-(7-azobenzotriazole)-N,N,N',N'-tetramethyluronium hexafluorophosphate and diisopropylethylamine in THF solvent at 10-30 DEG C for 12-30 h, and then carrying out post-treatment to obtain the bile acid-norfloxacin compound. The bile acid-norfloxacin compound is obtained by condensation reaction between the carboxyl group of the bile acid and the piperazine group of the norfloxacin, and the compound structure is combined with the bile acid and the norfloxacin. The antibacterial activity of the norfloxacin is obviously improved, the norfloxacin has better inhibition effect on Escherichia coli, Helicobacter pylori and the like, and also has better inhibition effect on Pseudomonas aeruginosa, Staphylococcus aureus and Pneumococcus, and meanwhile, the preparation operation process is simple.

The application belongs to the technical field of organic synthesis, and specifically provides a 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate, a preparation method and a condensation reagent. The preparation method of the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate comprises: making 2-chloro-4,6-dimethoxy-1,3,5-triazine and tetramethylurea undergo a nucleophilic substitution reaction to generate an intermediate; and making the intermediate and potassium hexafluorophosphate undergo an ion exchange reaction to generate the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate. The 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate according to the embodiment of the application can be used as a condensation reagent for forming an amide bond, and compared with condensation reagents such as HBTU and HATU which have two high-energy heteroatomic bonds of N-N and N-O, the thermal hazard of the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate is smaller, and the 2-(4,6-dimethoxy-1,3,5-triazin-2-yl)-1,1,3,3-tetramethylurea hexafluorophosphate is suitable for industrial production. In addition, the preparation method according to the embodiment of the application has mild reaction, fewer reaction steps and low operation risk coefficient.

The invention discloses a preparation method and application of sesamin targeted carrying nanoparticles, and the preparation method comprises the following steps: reacting ketal thiol TK, 2-succinimido-1, 1, 3, 3-tetramethylurea tetrafluoroborate, N, N-diisopropylethylamine and iramitide SS-31 peptide to prepare an SS31 peptide-TK compound, then reacting with chitosan, and simultaneously preparing a sodium alginate-lactobionic acid compound, so as to obtain the sesamin targeted carrying nanoparticles. Finally, mixing the two solutions to obtain a covalent complex; the method comprises the following steps: baking pork slices, extracting with ethanol, filtering, carrying out rotary evaporation, extracting, dialyzing and purifying, and freeze-drying; and mixing the products of the first two steps, dissolving in ethanol, adding sesamin, and carrying out electrostatic self-assembly and freeze drying to obtain the visual sesamin targeted nanoparticles. According to the invention, specific positioning of liver mitochondria, ROS stimulation response intelligent drug release and real-time visualization of food-borne fluorescence labeling are realized, and the application prospect in prevention and treatment of liver diseases is wide.

The application belongs to the technical field of magnesium ion batteries, and discloses a kind of aqueous magnesium ion battery electrolyte and its preparation method and application, the mixed electrolyte for aqueous magnesium ion battery is composed of magnesium salt, organic solvent and deionized water;Wherein, the organic solvent is tetramethyl urea (TMU), and tetramethyl urea and deionized water jointly constitute the mixed solvent of the mixed electrolyte, and the volume percentage of tetramethyl urea in the mixed solvent is 10%~50%, and the volume percentage of deionized water is 90%~50%;Magnesium salt is dissolved in the mixed solvent.The application improves the components of electrolyte, the mixed electrolyte with TMU as cosolvent and accurate control of TMU volume fraction, solves the problem of narrow electrochemical stability window (ESW) of aqueous magnesium ion battery, serious interface side reaction leads to the poor cycle life, and the electrolyte has the advantages of simple preparation, environmental friendliness and low cost, which provides a new way for improving the energy density and cycle life of aqueous magnesium ion battery.

The invention belongs to the technical field of organic synthesis, and particularly provides 2-(4, 6-dimethoxy-1, 3, 5-triazine-2-yl)-1, 1, 3, 3-tetramethylurea hexafluorophosphate, a preparation method and a condensation reagent. The preparation method of the 2-(4, 6-dimethoxy-1, 3, 5-triazine-2-yl)-1, 1, 3, 3-tetramethylurea hexafluorophosphate comprises the following steps: carrying out nucleophilic substitution reaction on 2-chloro-4, 6-dimethoxy-1, 3, 5-triazine and tetramethylurea to generate an intermediate; and carrying out ion exchange reaction on the intermediate and potassium hexafluorophosphate to generate 2-(4, 6-dimethoxy-1, 3, 5-triazine-2-yl)-1, 1, 3, 3-tetramethylurea hexafluorophosphate. The 2-(4, 6-dimethoxy-1, 3, 5-triazine-2-yl)-1, 1, 3, 3-tetramethylurea hexafluorophosphate provided by the embodiment of the invention can be used as a condensation reagent for forming an amido bond, and compared with condensation reagents with two high-energy heteroatom bonds of N-N and N-O, such as HBTU and HATU, the 2-(4, 6-dimethoxy-1, 3, 5-triazine-2-yl)-1, 1, 3, 3-tetramethylurea hexafluorophosphate is smaller in heat hazard and suitable for industrial production. In addition, according to the preparation method of the embodiment of the invention, the reaction is mild, the reaction steps are few, and the operation danger coefficient is low.

The invention discloses a preparation method of a tetrazine functionalized silk fibroin patch, which comprises the following steps: dissolving succinic anhydride in dimethyl sulfoxide, sequentially adding 4-dimethylaminopyridine and triethylamine, immersing a patch formed by spinning silk into the dimethyl sulfoxide, reacting at 35-40 DEG C for at least 6 hours, filtering, washing, and drying to obtain the tetrazine functionalized silk fibroin patch. After the reaction is finished, carrying out ultrasonic rinsing by using ethanol, a phosphate buffer solution and deionized water, and drying to obtain a carboxyl derivatization silk fibroin patch; the amount of succinic anhydride is at least 100 [mu] mol / cm < 2 >; dissolving a tetrazine compound in dimethyl sulfoxide, sequentially adding benzotriazole-N, N, N '-tetrazole-1, 2, 4-triazole, and reacting for 2-3 hours; the preparation method comprises the following steps: adding a tetrazine compound, N, N ', N'-tetramethylurea hexafluorophosphate and N, N-diisopropylethylamine, soaking the carboxyl-derived silk fibroin patch prepared in the step (1) into the mixture, reacting at 35-40 DEG C for at least 4 hours, ultrasonically rinsing by using ethanol, a phosphate buffer solution and deionized water after the reaction is ended, and drying to obtain the tetrazine-functionalized silk fibroin patch, with the dosage of the tetrazine compound being at least 50 mu mol / cm < 2 >.

The invention belongs to the technical field of organic synthesis, and discloses a vitamin A palmitate synthesis method, which comprises: carrying out a condensation reaction on retinol and palmitic acid according to a ratio under the combined action of a dehydrating agent and a nucleophilic catalyst at a condensation reaction temperature of 0-70 DEG C; the dehydrating agent is selected from dicyclohexylcarbodiimide, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride, 1-hydroxybenzotriazole or 2-(7-azabenzotriazole)-N, N, N ', N'-tetramethylurea hexafluorophosphate, and the solvent is selected from the group consisting of a solvent, a solvent and a solvent; the nucleophilic catalyst is selected from triethylamine, diisopropylethylamine, imidazole, 4-dimethylaminopyridine or 1, 8-diazabicyclo undec-7-ene, and the catalyst is one or more selected from the group consisting of 1, 8-diazabicyclo undec-7-ene. The method is simple to operate, mild in reaction condition, high in product yield and purity and suitable for industrial production.