68results about How to "Avoid harsh reaction conditions" patented technology

The invention relates to a preparation method of 2, 5-disubstituted thiophene compound I and the usage of the 2, 5-disubstituted thiophene compound in preparation of compound V. The preparation method is used for synthesizing the compound I by a 'one-pot' method through compound II and compound III under the condition that sulfur reagent exists. Compared with the prior art, the invention has the advantages of being easy in material obtaining, mild in reaction condition, simple and convenient in operation, high in yield, suitable for industrialized production and the like.

The invention provides ion liquid composed of fluoroalkyl sulfimide salt alkali metal salt containing 'S-fluoroalkyl sulfimide group', fluoroalkyl sulfimide negative ions containing 'S-fluoroalkyl sulfimide group' and positive ions of sulfonium salt, ammonium salt and microcosmic salt. The ion liquid utilizes (fluoroalkyl sulfonyl) (fluoroalkyl sulfinyl) imine with sulfur valence state as +4 and hydroxylamine oxygen sulfonic acid to react to prepare intermediate fluoro alkyl (S- fluoroalkyl sulfimide group) sulfamide of fluoroalkyl sulfimide, effectively shortens the line that the (fluoroalkyl sulfonyl) (fluoroalkyl sulfinyl) imine is utilized to prepare fluoro alkyl (S- fluoroalkyl sulfimide group) sulfamide of fluoroalkyl sulfimide through the three steps of chlorination, fluorination and amination, and is convenient to operate and high in yield and purity. The alkali metal salt has good heat stability and hydrolysis resistance, has high conductivity and oxidation potential in traditional carbonic ester solution, and is good in compatibility with electrode materials widely used. The ion liquid can be applied to lithium ion batteries and carbon-based super capacitors.

The invention discloses a method for preparing nano diamonds by using a direct-current arc process, belonging to the technical field of preparation of carbon-related nano materials. The method is characterized in that direct-current arc hydrogen plasma is used as a heat source, graphite is used as a carbon source, nickel is used as a catalyst and silicon is used as a nucleation substance to synthesize diamond nano-particles. High-temperature hydrogen plasma is used for evaporating a block composite target material to form atomic and ionic states of raw material components, a silicon carbide cluster crystal nucleus is formed and atoms are induced to form a diamond phase during condensation, carbon atoms separated out from a supersaturated nickel-carbon solid solution become growth substances for the diamond phase, and a nano diamond blank is obtained through passivation. The remaining impurities including metals, graphite, amorphous carbon, silicon carbide and the like are removed through purification processes including acid treatment, high-temperature oxidation, rinsing and the like so as to obtain high-purity diamond nano-particles. The method disclosed by the invention has the effects and benefits that the preparation process is simple, the synthesis is performed under a normal pressure condition, and the low cost, low energy consumption and large-scale production of the diamond nano-particles are realized.

The invention discloses a method for preparing a metal nanomaterial with a simulated cell structure, which is characterized by comprising the following steps of: reducing metal ions in an external metal salt solution on surfaces of metal nanoparticles by using a reducing agent for forming a core-shell structure to form a binary metal core-shell structure; reducing high-valence metal ions in a subsequently added metal salt solution into middle and low-valence metal ions on the surface of the binary metal core-shell structure by using a reducing agent for forming the simulated cell structure; and sacrificing a metal shell through displacement reaction between two kinds of metal to form a simulated cell metal nanostructure consisting of a metal core, a cavity and metal walls. The severe condition required by the conventional single high-temperature metal displacement reaction is avoided, the shape of the original nanometal core can be completely kept, and the nanometal material of which the inner cavity contains the movable metal core is formed; and the metal nanomaterial can be applied to fields of environment detection, industrial catalysis, biomedicine and the like and is high in universality, and the preparation method is simple.

The invention relates to synthesis method for industrial production of octreotide. The method is characterized by comprising the following steps of: 1. taking aminomethyl resin as the starting resin, utilizing condensation reagents HOBT and DIC to couple the raw material Fmoc-Thr-x to the resin to generate Fmoc-Thr-x AM Resin; then coupling amino acids Cys, Thr, Lys, Trp, Phe, Cys and Phe to Fmoc-Thr-x AM Resin one by one in order, thus obtaining octreotide peptide resin; 2. adding a lysate solution, stirring the substances evenly and performing cracking for 2-3h; 3. dissolving octreotide crude peptide into a TFA/water mixed solution, then putting the mixture into 35DEG C-38DEG C water bath to perform heating for 2-3h to make the linear peptide of octreotide have single peak pattern in HP LC chromatogram; and 4. adding DMSO, then performing oxidation for 1-1.5h, conducting HPLC detection of a cyclization end point, and performing separation and purification to obtain a refined product of octreotide. In short, the synthesis method provided by the invention has simple technique, and is suitable for industrial production. After post-treatment, the HPLC peak pattern of octreotide crude peptide is simple, the cyclization method is easy to operate, cyclization is complete, the yield is high and the purity is 98% or more.

The present invention discloses a module compound with hydrogen bond sequence specificity combination and a preparation method thereof. The structure formula of the compound module is as follows: wherein, when R is (m is any integer of 1-200), the module compound is a hydrophilic module compound P2; when R is (n is any integer of 2-140), the module compound corresponds to the hydrophobic module compound of BLOCK-1, BLOCK-2 or BLOCK-3. As the module compound has hydrogen-sequence specificity and the two complementary single-stranded can mutually recognize and match with specificity, the block copolymer which is not easy to synthesize by other methods can be easily prepared by using a molecular glue group.

The invention relates to a synthesis method of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride, which comprises the following steps: reacting a compound (3) and fluorobenzyl bromide in the presence of DMF (N,N-dimethylformamide) and potassium carbonate to obtain a compound (4); dissolving the compound (4) in absolute methanol, adding sodium methoxide, stirring and reacting to obtain a solution containing a compound (5); and reacting the solution containing the compound (5) with ammonium chloride and glacial acetic acid, and salifying with hydrogen chloride. The synthesis method provided by the invention has the advantages of cheap raw materials, mild reaction conditions and high total yield, is simple to operate, and is suitable for large-scale synthesis of the important intermediate 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridyl-3-formamidine hydrochloride of riociguat for treating adult chronic thromboembolic pulmonary hypertension (CTEPH) and pulmonary artery hypertension (PAH).

The invention discloses a method for synthesis of xylosic acid by biological catalysis of D-xylose. The method comprises the following steps: A) constructing a recombinant engineering receptor bacteria strain which is capable of converting the D-xylose to the xylosic acid and contains a xylose dehydrogenase gene xylB gene fragment and a xylose acid lactonase gene xylC gene fragment; and B), using the engineering receptor bacteria in the A for fermentation cultivation in a D-xylose-containing culture medium, using an appropriate inducer for introduction, and separating and purifying to obtain the xylose acid.

The invention relates to a method for preparing gamma-GVL by homogeneous catalysis. According to the method, levulinic acid esters are taken as raw materials, secondary alcohols are taken as hydrogen sources and solvents, and in the catalysis of aluminium isopropoxide, hydrogen transfer and lactonization are carried out to obtain the gamma-GVL. The method for the high-selectivity preparation of the gamma-GVL by the homogeneous catalysis has the advantages of short reaction time, fast substrate conversion, high conversion rate, high product selectivity and almost no side reaction. The method does not require high-pressure hydrogen in the reaction process, thereby not needing to isolate air; used catalysts are non-noble metal catalysts, so that the prices are low; harsh reaction conditions of requirements on high temperature and high pressure, protection of inert gases and use of noble metal catalysts are avoided in the existing preparation process, and the method disclosed by the invention is mild in reaction conditions, low in equipment requirements, simple in process and convenient to operate. The secondary alcohols in the method can be recycled. The safety and economy of the preparation method are improved.

The invention discloses a linear tin phosphide compound. A chemical formula of the linear tin phosphide compound is Sn4P3; the linear tin phosphide compound has a linear shape and has the length of 0.1mu m to 12mu m and the length-width ratio is 1 to (1.82 to 35.7). The linear tin phosphide compound is prepared by adopting the following steps: carrying out high-energy ball milling on red phosphorus, tin powder and aluminum powder; carrying out calcination on the obtained powder in a vacuum tubular furnace to obtain the linear tin phosphide compound. According to a preparation method of the linear tin phosphide compound, disclosed by the invention, the production cost is reduced, a generation procedure is greatly simplified, the production time is shortened and the yield is improved. Meanwhile, harsh reaction conditions including a toxic phosphorus source, high pressure and the like are also avoided. A prepared phosphide has a linear structure so that the specific surface area is greatly improved, hydrodesulfurization (HDS), hydrodenitrogenation (HDN) and hydrodeoxygenation (HDO) activity and photocatalysis performance of the phosphide are improved and application performance of the phosphide in a lithium-ion battery material is improved.

The invention discloses a preparation method of 1,2,3-bis-triazole ligands and an application of the 1,2,3-bis-triazole ligands in a CuAAC reaction. With cheap and easily available glycine methyl ester hydrochloride as a base raw material, and through derivation and conversion of functional groups, a diyne compound with glycine as a structure is obtained; then under a condition of room temperature and with organic azide as a raw material and copper iodide as a catalyst, 1,2,3-bis-triazole seven-membered-ring compounds are synthesized; and with the bis-triazole compounds and derivatives thereof as substrates, a series of methods for synthesis of the 1,2,3-bis-triazole derivatives are developed. A variety of novel, highly efficient, simple and easily available ligand catalysts are provided for a click reaction, and the 1,2,3-bis-triazole ligands have obvious effect on accelerating the reaction when used as the ligands and have quite practical application.

The invention provides a preparation method of a catalyst for preparing methanol by low-temperature plasma-optical coupling methane and a method for preparing methanol. The method comprises the following steps: adding 0-20mg of a Cu-C catalyst into 1-5mL of water, carrying out uniform ultrasonic dispersion so as to obtain a mixed solution, pouring the mixed solution into a DBD reactor, and carrying out a reaction under normal temperature and normal pressure so as to obtain the methanol wherein the flow rate of CH4 is 5-30mL/min, and the discharge power is 5-50W. According to the method, low-temperature plasma is adopted to catalyze CH4 and H2O to prepare methanol through one-step conversion, H2O which is low in price and easy to obtain is selected as an oxidizing agent, excessive oxidationof CH4 is restrained, H2O can serve as an absorbent, generated CH3OH is transferred into a liquid phase in time, and decomposition of products is effectively restrained. As the plasma can generate high-energy electrons, CH4 can be activated at normal temperature and normal pressure, and harsh reaction conditions are avoided.

The invention discloses a preparation method of 3-substituted phenyl-5-(aminomethyl) oxazolidin-2-one. The preparation method comprises the following steps of: enabling substituted aniline to react with (R)-chloro-epoxy propane to get (R)-3-substituted phenylamino-2-hydroxy-chloropropane, further reacting with dibenzyl amine to get (R)-3-substituted phenylamino-1-dibenzyl amino-2-propanol, cyclizing to get (S)-3-substituted phenyl-5-dibenzyl aminomethyl oxazolidin-2-one and finally performing hydrogenation and debenzylation to get (S)-substituted phenyl-5-(aminomethyl) oxazolidin-2-one. A compound obtained by the method disclosed by the invention is of an important intermediate for commercial production of oxazolidinone type antibacterial agents. The method for preparing the 3-substituted phenyl-5-(aminomethyl) oxazolidin-2-one through four-step reaction has the characteristics of few steps, simple operation, low cost and easiness in obtainment of raw materials, mild reaction conditions and the like; and by adopting the method, the production efficiency can be improved, the production energy consumption can be reduced, a safety production coefficient can be further improved, environmental pollution can be reduced, and the preparation method is of an environment-friendly and low-carbon green synthesis method.

The invention discloses a preparation method of 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone. The preparation method comprises the following steps: carrying out condensation reaction on substituted aniline which is used as a starting material and 3-sustituted-1,2-propanediol so as to synthesize an intermediate (R)-(+)-3-substituted phenylamino-1,2-propanediol; and preparing 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone through two-step reaction, wherein the obtained product 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone is an important intermediate used for commercially producing oxazolidinone antibacterial agents. The method for preparing 3-substituted phenyl-5-hydroxymethyloxazolidine-2-ketone through two-step reaction has the characteristics of less steps, cheap and available raw materials, mild reaction conditions and the like, and is simple to operate; and by using the method in the invention, production efficiency is improved, production energy consumption is reduced, safe production coefficient is improved, production cost is reduced, environment pollution is reduced, thus the method in the invention is an environmentally-friendly low-carbon green synthesis method.

The invention provides a bimetallic compound sulfonate with high alkalinity, sodium and magnesium containing alkylbenzenesulfonate, the preparing method, and the application of said bimetallic compound sulfonate as lubricant additive. The said sulfonate is characterized by good anti-extreme pressure, anti-oxygen and cleaness, high total alkalinity and adjustable sodium and magnesium content. The method comprises following steps: mixing alkylbenzene sulfonic acid, sodium alkali compound, magnesium alkali compound with low carbon alchol, water, diluting oil and accelerator for reaction; feeding carbon dioxide for carbonation, separating and getting final product. The content of said bimetallic compound sulfonate used as lubricatant additive in oil should be less than 5% by weight.

The invention discloses a novel C8-heterocyclic alkylated purine nucleoside analogue and a synthetic method thereof and provides a method for synthesizing a C8-heterocyclic alkylated nucleoside analogue by high-efficiency C-H activation. The method adopts raw materials which are easily available, and is moderate in reaction condition and few in reaction steps. The method aims to solve the problems of expensive raw materials, complex process and harsh reaction condition during synthesis of the type of compound, to provide a reference value for synthesis and application of a nucleoside medicine and to provide the raw materials for research of novel anti-virus and antitumor drugs. Meanwhile, the method disclosed by the invention provides an effective method for heterocyclic alkylatation of other nucleosides and analogues of the nucleosides and is wide in industrial application prospect.

The invention discloses a synthesis method of a Frutinone compound, which comprises the following steps: (1) under the action of Cs2CO3 and a base, substituted ethyl benzoylacetate and substituted 2-chlorobenzoyl chloride react to obtain intermediate 1; (2) the intermediate 1 and boron trihalide are subjected to a hydrolysis reaction to obtain the intermediate 2; (3) the intermediate 2 is oxidizedwith potassium persulfate to obtain a target product. The substituted ethyl benzoylacetate, the substituted 2-chlorobenzoyl chloride, Cs2CO3, boron trihalide and potassium persulfate are used as themain raw materials, and the raw materials are cheap and easy to obtain, thus avoiding the expensive raw materials or precious metal catalysts involved in the existing methods; the synthesis method hasthe advantages of simple operation, mild reaction conditions, environmental friendliness, easy solvent recovery and application, and is suitable for industrial production.