46results about How to "Mild reaction conditions" patented technology

The invention discloses a preparation method for a beta-amido-alpha-amino-acid ester derivative. The preparation method includes the steps of having a reaction in organic solvent under the nitrogen atmosphere till a substrate is completely converted with heavy-nitrogen derivatives and aminal derivatives as starting raw materials and Lewis acid as catalysts; pumping out all the solvent after the reaction ends, and conducting preparative chromatography to obtain the beta-amido-alpha-amino-acid ester derivative. Under catalysis of the various Lewis acid catalysts, heavy-nitrogen compounds and aminal compounds react in two groups, the beta-amido-alpha-amino-acid ester derivative can be further efficiently prepared, the Lewis acid catalysts and raw materials of the reaction are low in price and easy to obtain, and the synthesis process is simple.

The invention discloses a preparation method of a hydrophobic graphene conductive material. The preparation method specifically comprises the following steps: (1) adding graphene oxide into a CH3CN solution for ultrasonic dispersion; (2) sequentially adding an alkaline reagent, a photocatalyst and a fluorinating reagent, uniformly stirring, reacting under illumination, filtering, washing, and freeze-drying; and (3) adding into deionized water for ultrasonic dispersion, adding hydrazine hydrate, uniformly mixing, stirring for reaction, filtering, washing and drying, thereby obtaining the product. The invention also discloses a preparation method of the hydrophobic conductive flexible composite film, and the preparation method specifically comprises the following steps: adding the hydrophobic graphene conductive material into a DMF solution for ultrasonic dispersion, then adding TPU particles for swelling, stirring until the TPU particles are uniformly mixed after the TPU particles are completely swelled, coating a smooth glass plate with the mixture, and drying to obtain the hydrophobic conductive flexible composite film. The reaction can be carried out at normal temperature and normal pressure under the photocatalytic condition, and the reaction condition is mild; the conjugated structure of the graphene is not damaged, and the prepared product has good hydrophobic and conductive performance.

The invention discloses a preparation method of nitrogen-doped TiO2 powder and belongs to the technical field of materials. The preparation method comprises the following steps: firstly, dropwise adding tetramethylammonium hydroxide into absolute ethyl alcohol and stirring to obtain a mixed solution; secondly, dropwise adding titanium isopropoxide into the mixed solution to obtain sol; thirdly, immersing a copper plate into the bottom of the sol, drying the copper plate at the temperature of 60 to 80 DEG C after the copper plate is aged and taking out; fourthly, conducting direct current to the copper plate and sintering colloid on the surface by utilizing the heating of the copper plate; fifthly, scrapping the sintered material on the surface of the copper plate after sintering is finished, wherein the scraped material is the nitrogen-doped TiO2 powder. The preparation method of the nitrogen-doped TiO2 powder, disclosed by the invention, has the advantages of simple synthetic processand mild reaction conditions; in addition, the sintering time of a sample is greatly shortened; the sintered sample has better shape and the structure is more stable; besides, the degradation rate ofthe prepared nitrogen-doped TiO2 to methylene blue is significantly increased.

The invention provides a cadmium-ion fluorescence probe based on a pyrene exciplex, and a preparation method and application thereof. The probe has a structure as described in the specification. The preparation method comprises the following steps: dissolving 1-aminopyrene in CH2Cl2, then adding DMAP and slowly adding chloroacetyl chloride drop by drop under an ice-bath condition; allowing the temperature of a mixture obtained in the previous step to slowly rise to room temperature, removing the solvent through rotary evaporation after completion of a reaction, and loading a reaction product into a silica gel column; adding acetonitrile into obtained 1-(2-chloroacetyl)pyrene, then adding KI and DIPEA and slowly adding DPA drop by drop; and carrying out a reflux reaction, carrying out spin-drying to remove the solvent after completion of the reaction and treating a product of the reflux reaction with the silica gel column. The probe provided by the invention can emit fluorescent response signals specific to cadmium ions and is applicable to detection of cadmium ions in environment.

The invention provides a preparation method of trans-cyclobutane o-dicarboxylic acid ester and a derivative thereof. The preparation method comprises: in an organic solvent, catalyzing a substrate with a structure represented by a structural formula I by utilizing an organic alkali at 50-90 DEG C to generate isomerization so as to obtain trans-cyclobutane o-dicarboxylic acid ester or a derivativethereof, wherein the structural formula I is defined in the specification, R<1>, R<2>, R<3> and R<4> are respectively and independently hydrogen or any one selected from C1-C5 alkyl, and R<5> and R<6>are respectively and independently any one selected from C1-C10 alkyl and benzyl. According to the invention, by using the organic alkali as the catalyst to catalyze the isomerization reaction of thetrans-cyclobutane o-dicarboxylic acid ester with the structural formula I or the derivative thereof at 50-90 DEG C, the one-step isomerization shortens the process steps, is efficient and simple, hasmild reaction conditions, and does not need special equipment, so that the scale-up production is easily achieved, and the substrate conversion rate of more than 70% even more than 80% and the product yield of more than 70% or even more than 80% can be achieved in the scale-up production.

The invention discloses a phthalate type plasticizer hydrogenated catalyst preparation method thereof and an application, and belongs to the field of catalytic hydrogenation. The catalyst consists of active component, assistant and carrier, wherein the active component is 0.1-3% of total content of catalyst by mass, assistant is 1-10% of total content of catalyst by mass, and the rest is carrier. The active component of the catalyst is precious metal element ruthenium; assistants are copper, manganese, cobalt, nickel, iron, chromium and tin; the carrier is zirconia, titanium oxide, alumina, silica, silicon carbide, zinc oxide, magnesium oxide, activated carbon, diatomite, aluminosilicate, molecular sieve. Compared with the prior art, the catalyst preparation method is simple in preparation, gentle in reaction condition, high in product yield, and free from side product.

The invention belongs to the technical field of medicinal chemistry, in particular to an amisulpride impurity and a preparation method thereof. The preparation method comprises the following steps: inthe co-existence of a condensing agent and an activating agent, a compound I is subjected to a self-condensation reaction at the temperature of 10-70 DEG C, and a compound crude product shown as a formula (II) is prepared, wherein the molar ratio of the compound I to the condensing agent is 1: (0.4-0.7), the molar ratio of the compound I to the activating agent is 1: (0.4-0.7), and the specific is shown as follows.

The invention discloses a preparation method of N epsilon-tert-butoxycarbonyl-N alpha-fluorenylmethoxycarbonyl-N epsilon-methyl-lysine. The preparation method comprises the following steps: taking N alpha-fluorenylmethoxycarbonyl-lysine hydrochloride as a raw material, performing alkylation with halide (R-X) under alkaline conditions, performing reductive amination on alkylate in an aqueous formaldehyde solution to introduce methyl, removing an R group of a reductive amination product under acidic conditions, then introducing a t-butyloxycarboryl (BOC) protecting group under alkaline conditions and performing re-crystallization treatment to obtain a product. The preparation method disclosed by the invention is simple in synthetic route and mild in reaction conditions, and the next-step reaction can be directly carried out after an intermediate is simply washed and concentrated. The reaction yield in each step is close to quantification, the total yield can reach above 80 percent, the purity of a final product exceeds 98 percent, and a safe and efficient synthetic route is provided for the preparation of the N epsilon-tert-butoxycarbonyl-N alpha-fluorenylmethoxycarbonyl-N epsilon-methyl-lysine.

The invention discloses a method for preparing an intermediate of chiral vicinal diamine. The method comprises the following steps: adding a compound IV into a solvent, stirring the compound IV and the solvent in an ice water bath, adding an initiator into the obtained reaction system, adding a reducing agent into the reaction system in batches, heating the reaction system to 20-80 DEG C, and stirring the reaction system; and extracting the reaction system after the reaction is completed, drying the obtained organic phase, filtering the dried organic phase, and performing rotary drying to obtain a compound V that is the intermediate. The preparation method of the invention has the advantages of simplicity and mild reaction conditions, and can be widely applied to industrial production.

The invention discloses a low-silver-content fish scale gelatin-agar-Ag NPs composite film as well as a preparation method and application thereof, belongs to the technical field of functional nano materials, and provides a preparation method of a low-silver-content fish scale gelatin-agar-Ag NPs composite film, which comprises the following steps of: reacting fish scale gelatin serving as a reducing agent and a stabilizing agent with silver ammonia ions to prepare Ag NPs; and mixing Ag NPs with a fish scale gelatin solution and an agar solution, and conducting treatment through a solution pouring method, so as to prepare the low-silver-content fish scale gelatin-agar-Ag NPs composite film. The invention also aims at providing application of the low-silver-content fish scale gelatin-agar-Ag NPs composite film to packaging or film liquid coating preservation of vegetables, fruits, food and the like.

The invention belongs to the technical field of chemical synthesis of drugs, and particularly relates to a novel synthesis process method of a nitroimidazole pyran drug for treating tuberculosis with wide drug resistance. The preparation method comprises the following steps: taking 2-bromo-5-nitro-1H-imidazole and glycidyl butyrate as initial raw materials, and obtaining (S)-3-(2-bromo-4-nitro-1H-imidazole-1-yl)-2-hydroxypropyl butyrate (an intermediate I) under the condition of N, N-diisopropylethylamine and methylbenzene; the preparation method comprises the following steps: redissolving by using acetonitrile, and stirring and reacting with 4-trifluoromethoxy benzyl bromide at room temperature in the presence of cesium carbonate to obtain (S)-3-(2-bromo-4-nitro-1H-imidazole-1-yl)-2-(4-(trifluoromethoxy) benzyl) oxy) propyl butyrate (intermediate II); the invention discloses a synthesis method of (S)-6, 7-dihydro-2-nitro-6-[[4-(trifluoromethoxyl) phenyl] methoxyl]-5H-imidazo [2, 1-B] [1, 3] oxazine, namely pretomanid, and the synthesis method is simple in route step and high in product yield. Experiments prove that the product has good safety and effectiveness, and a feasible synthesis route scheme is provided for industrial production of the pertomanib.

The invention belongs to the technical field of organic chemical synthesis, and discloses a 5,5'-bitetralone chiral skeleton, a chiral phosphoric acid with the 5,5'-bitetralone skeleton, and a method for preparing the chiral phosphoric acid on the basis of 5,5'-bitetralone-6,6'-diphenol and substitutes thereof. The phosphoric acid maintains the advantages of favorable enantioselectivity in the chiral phosphoric acid based on BINOL and H8-BINOL in tradition, and also has excellent enantioselectivity in some organic reactions. The chiral phosphoric acid with the 5,5'-bitetralone skeleton overcomes the defect of lower catalytic activity, and has higher reaction activity than the traditional phosphoric acid. The preparation method has the advantages of cheap and accessible raw materials and catalyst, shorter synthesis route, simple technique and mild conditions, and has industrialization potential.

The invention discloses a whole aqueous phase synthetic craft of medical intermediate methyl-dithioic acid, which comprises the follwing steps: using calcium cyanamide, soda and carbon bisulphide for raw material; adding in phase transition accelerant to generate dithioic acid disodium salt; getting dimethyl-dithioic acid treated by methylating agent-dimethyl sulfate. The invention reduces the cost, which relizes the industrialization production.

The invention belongs to the technical field of catalytic chemistry and environmental protection, and relates to a deep desulfurization method for 380-780 nm visible light catalytic oxidation diesel oil. The desulfurization method comprises the following steps: 1, preparing a heteropolyacid-loaded TiO2 catalyst; and 2, adding the catalyst into diesel oil, and carrying out photocatalytic oxidationdesulfurization under the condition of 380-780nm visible light. According to the method disclosed by the invention, a heteropolyacid-loaded TiO2 nano material is used as a catalyst, so that the problems that a titanium dioxide material is used as a diesel photocatalytic oxidation desulfurization catalyst, the energy utilization under visible light in a sunlight region is less, and the photocatalytic efficiency is low due to a serious photo-induced electron and hole compounding phenomenon are solved. The invention is used for visible light catalytic oxidation desulfurization of model diesel oil. The technological process is simple to operate, the reaction conditions are mild, and the catalyst can be recycled. The catalytic activity of the desulfurization reaction is very high, and the desulfurization rate is up to 100%.

The invention discloses an organic compound for detecting content of metal ions in water environment. According to the organic compound, N, N-methylpyridine aniline serves as a metal ion complex, chromophore or fluorophore is introduced to the molecule of the compound, so that an color indicator or fluorescent indicator of metal ions, especially cadmium ion and zinc ion is obtained. The compound can be fixed to hydrophilic polymers, and can be prepared into reversible metal ion fluorescent probe which is reusable according to characteristics of the chromophore or fluorophore; the reversible metal ion fluorescent probe is applicable to continuous detection of concentration of metal ions in various environments, especially to continuous detection of concentration of cadmium ion and zinc ionin the water environment.

The invention discloses a preparation method of a [1, 2, 4] oxadiazino indoline-3-ketone derivative, which comprises the steps of (1) mixing an o-nitrophenylacetylene compound, a catalyst and a first organic solvent, and reacting at room temperature for 3-6 hours; and (2) adding an alpha-halogenated hydroxamic acid ester compound, sodium carbonate and hexafluoroisopropanol into the material obtained in the step (1), and reacting at room temperature for 10-12 hours; or mixing the o-nitrophenylacetylene compound, the catalyst, the alpha-halogenated hydroxamic acid ester compound, sodium carbonate and hexafluoroisopropanol, and reacting at the temperature of 55-65 DEG C for 10-12 hours. According to the invention, the [1, 2, 4] oxadiazino indoline-3-ketone derivative having a variety of substituents, which is difficult to synthesize by other methods, can be synthesized, and the method has profound significance in the aspect of organic chemistry.

The present invention discloses a synthesis method of an alpha-aminoacid derivative substituted by an alpha-alkyl branch. The method comprises the following steps: olefin reacting with 9-bbn at 0-80 DEG C for 0.5-12 h; then adding imine; in the presence of a transition metal salt, an alkali and an organic solvent, performing reacting at 0-90 DEG C for 12-48 h to produce the alpha-aminoacid derivative. According to the present invention, an alkyl boron reagent is produced in a situ manner by using olefin and 9-bbn, the reaction condition is mild, and a variety of olefin may be selected. In addition, the existing synthesis method needs the strict anhydrous oxygen-free condition, the reaction manipulation is complex, the reaction needs to be performed at a low temperature, and the cooling cost is high. However, according to the method, the anhydrous oxygen-free condition is not needed, and the reaction may be performed at the room temperature or at a slightly higher temperature.

The invention provides a method for recycling utilization of epoxy chloropropane oil layer rectifying still residues, and particularly relates to a method for preparing glyceryl ether by taking the epoxy chloropropane oil layer rectifying still residues and methanol as raw materials and taking acidic ionic liquid as a catalyst. By selecting a proper catalyst, the epoxy chloropropane oil layer rectification kettle residue is converted into glyceryl ether; the reaction condition is mild, the rectification kettle residue resource utilization is realized, and the production cost is reduced.

The invention discloses a green synthesis method of drug active molecules GC-24 and furegrelate. From the perspective of the structure, the GC-24 and furegrelate contain a diaryl methanestructure. Benzyl alcohol and an aryl electrophilic reagent which are cheap and easy to obtain are used as raw materials, dimethyl oxalate (33 yuan/100 g) is used as an activating agent, and a key framework is constructed in one step by utilizing a reductive coupling strategy under the catalysis of nickel. Operation is simple, and synthesis is convenient. Compared with the existing optimal preparation method, the synthesis of the GC-24 is reduced from 10 steps to 4 steps; strong corrosive and irritant chemicals such as HBr, BCl3 and the like, and expensive drugs such as palladium metal catalysts, carbene ligands and the like are prevented from being used. The synthesis of the furegrelate not only shortens the original preparation route by half, but also avoids the use of strong corrosive reagents such as nitric acid, sulfuric acid, trifluoroacetic acid and the like, and avoids the flammable and explosive processes such as catalytic hydrogenation, diazotization and the like. The synthesis method of the two drugs has good step economy and atom economy.

The invention relates to the technical field of biology, in particular to a compound for detecting copper ions and preparing a drug for preventing and treating Alzheimer disease, a preparation method of the compound and a product. The structural formula of the compound is as shown in a formula I or a formula II (as showed in the description). The product can be prepared from cheap and readily available raw materials through one-step synthesis under mild and simple reaction conditions, the two compounds have high selectivity to copper ions and detection limit up to nanomolar level, and can sensitively detect the change of the intracellular copper ion level; and besides, ligands can chelate copper ions, so as to effectively inhibit copper ion-induced cross-linking of amyloid beta-protein, and significantly reduce neurotoxicity caused by cross-linking of amyloid beta-protein, and therefore, the compounds have an important potential value in the field of research and development of Alzheimer disease drugs.

The invention discloses an all-new preparation method of a compound with a formula (I). The preparation method comprises the following steps: (1) carrying out esterification reaction on 9-fluoro-3,7-dihydro-3-methyl-10-(1-aminocyclopropyl)-7-oxo-2H-(1,4)oxazino(2,3,4-1)quinoline-6-carboxylic ethyl ester in a single-methanol solvent under the acid condition; and (2) applying DMF-DMA to carry out reductive amination reaction and hydrolysis reaction on products. The preparation method disclosed by the invention has the advantages of higher safety, simpler synthetic route, mild reaction conditions, easiness in operation, higher yield, applicability to industrial production and benefit for promotion and application of the compound with the formula (I).