510results about How to "The reaction is easy to operate" patented technology

The invention discloses a phenyl bistriazole compound, and a preparation method and application thereof, and particularly relates to a 1-[4-(1H-1,2,4-triazole-1-yl)phenyl]-1H-1,2,4-triazole single crystal and a preparation method of 1-[4-(1H-1,2,4-triazole-1-yl)phenyl]-1H-1,2,4-triazole. The organic compound is prepared by heating ethylenediamine, 1H-1,2,4-triazole, potassium carbonate, 1,4-diiodobenzene and cuprous iodide through a one-pot method. The preparation method disclosed by the invention has the characteristics simple process operation, low production cost and less environmental pollution, and is suitable for large-scale industrial production. The 1-[4-(1H-1,2,4-triazole-1-yl)phenyl]-1H-1,2,4-triazole single crystal prepared by the invention can be used in the aspect of photoelectric materials, especially dye and luminescent agents.

The invention provides a high temperature resistant Gemini cationic viscoelastic surfactant (VES) and a synthetic method thereof, relating to the field of oil recovery technology and engineering in the petroleum industry. The synthetic method is characterized by reacting unsaturated long-chain fatty acid with N,N-dimethyl propanediamine to synthesize a fatty acid amide intermediate; reacting methylamine with epichlorohydrin to synthesize a chloramine intermediate; reacting the intermediates synthesized in the two above steps respectively to synthesize the high temperature resistant Gemini cationic VES. The VES and the synthetic method have the beneficial effects that a high temperature surface active diverting acid system reacts with rocks at 160 DEG C, so that the liquid obviously diverts to become viscous and is subjected to automatic gel breaking under the condition that the hydrochloric acid concentration is below 5%, thus achieving rapid flowback; the VES has good temperature resistance, is relatively low in price and is beneficial for popularization and application.

The invention discloses a linaclotide solid-phase synthesis method, and belongs to the biochemical technical field. The method includes the following steps: (1) preparation of linaclotide resin; (2) cutting the linaclotide linear peptide resin obtained in the step (1), to obtain a protection group linear peptide containing Cys(Acm) and Cys(tBu); (3) oxidizing to form a first disulfide bond, to obtain a monodisulfide cyclopeptide; (4) removing an Acm protection group in the monodisulfide cyclopeptide, to obtain a dual disulfide cyclopeptide; (5) removing a tBu protection group of the dual disulfide cyclopeptide, to obtain a trisdisulfide cyclopeptide; and (6) purifying the trisdisulfide cyclopeptide by HPLC, and freeze-drying to obtain linaclotide. The process has the characteristics of simple reaction operation, easy post-processing, low cost, high yield, and considerable economic and practical values, and besides, has wide application prospect in the polypeptide drug design and synthesis field.

The invention discloses a method for preparing an organic ternary polycarboxylic acid dustless antirust additive 2,4,6-tri(amino caproyl)-1,3,5-triazine by adopting a one-pot method, which comprises the following steps of: ring-opening caprolactam with alkali to generate carboxylate of aminocaproic acid first; then performing a substitution reaction by the carboxylate of aminocaproic acid and cyanuric chloride; and finally, acidizing with hydrochloric acid to prepare derivatives of organic ternary polycarboxylic acid. The preparation method is free from a toxic organic solvent and employs common water as a solvent for reaction. The preparation method ha the advantages of simple process operation, low production cost and low environmental pollution and is more suitable for large scale industrial production.

A benzimidazole ester compound, 2-ethoxy-1-(p-halophenyl) methyl-1H-benzimidazole-7-carboxylate-1-[[(cyclohexoxy)carbonyl] oxy] ethylester, its preparing process, and its application in preparing medicinal compound candesartan ester are disclosed.

The invention relates to a method for synthesizing 6-methyl-17alpha-acetoxyl-19-norpregnane-4,6-diene-3,20-diketone. The method comprises the following steps: 1) reacting acetylene with estrone-3-methyl ether so as to obtain 17alpha-acetenyl estrone-3-methyl ether; 2) carrying out Birich reaction at a low temperature; 3) carrying out alkene etherification on the product obtained in the step 2); 4) carrying out a Vilsmeier reaction on the product obtained in the steps 3); 5) reacting the product obtained in the step 4) with benzene sulfenyl chloride; 6) reacting the product obtained in the step 5) with sodium methoxide and trimethyl phosphate; 7) reducing the formoxyl at the 6-position of the product obtained in the step 6); and 8) reacting the product obtained in the step 7) with Pd-C/cyclohexene, then reacting with acetic oxide so as to obtain the target product 6-methyl-17alpha-acetoxyl-19-norpregnane-4,6-diene-3,20-diketone. By using the method, the operation is simplified, and theproduction cost is reduced; and the reactions involved in the invention are simple to operate, and the yield is high.

A nano colloidal golf linked immunoassary for detecting carbofuran includes such steps as coupling the immunized semi-antigen of carbofuran with BSA, synthesizing artificial immunoantigen compound, immunizing animal to prepare specific high-valence BFNH antibody, separating and purifying, linking the nano-class colloidal golf to said specific antibody, solidifying said linked compound, carbofurancoupled by egg albumin and sheep's mouse IgG antibody on a carrier, and for semi-quantitative analysis. Its advantage is high sensitivity and speed.

The invention belongs to a test paper and a preparation method for quickly semi-quantitative testing the residual quantity of 2, 4-D in synthetic water samples, the invention relates to a GICA reaction which relies on a colloidal gold mark to show color, and the invention belongs to the immunochemistry measurement technical field. The theory of the invention is according to the reaction of 2, 4-D and the accurately quantitative gold mark antibody, and then the reactant has an emulous combination with the 2, 4-D-OVA which is cross-band-shaped distributed on the GICA film, and the content of the 2, 4-D of the sample is judged by the number of the stripe on the GICA film. The number is huge, the content of the 2, 4-D of the sample is high, the LOD of the 2, 4-D is 21ug/l, and the test can be finished in 10 minutes. The invention has practical character and remarkable progress, the traditional multi-step fussy detecting of the agricultural chemical is changed, and the method for quickly semi-quantitative testing the residual quantity of 2, 4-D in one-step is realized. The test paper stripe comprises a soleplate, an absorbent filter, a nitrocellulose membrane, a gold mark pad of anti-2, 4-D antibody and a sample adsorption pad, the nitrocellulose membrane in the middle of the soleplate is used for the experiment reacting region of a cellulose nitrate membrane, 4 detection lines and a quality control line are on the cellulose nitrate membrane, a sample area is on the far left, an absorbent filter is on the other end of the soleplate.

The invention relates to the field of pharmaceutical chemistry, in particular to a synthesis method of a minodronate midbody and synthesis of minodronate. The preparation method of minodronate includes the following steps: using organic solvent to dissolve 2-aminopyridine, adding 4-acetyl chloride ethyl acetoacetate for reaction, monitoring the reaction solution by TLC(Thin-Layer Chromatography) until spots of 4-acetyl chloride ethyl acetoacetate disappear, concentrating to a dry state, dissolving concentrate in water, washing a water layer to remove impurities, extracting the water layer with the organic solvent, washing extract liquor, separating out an organic layer, conducting filtration, and concentrating the concentrate to be in a dry state, thereby obtaining A1.

The present invention discloses a method for synthesis of acetal/ketal in presence of acidic ionic liquid as catalyst, including: taking aldehyde/ketone and alcohol as raw materials and cyclohexane as a dehydrating agent, and performing azeotropic dehydration condensation under the catalytic action of the acidic ionic liquid at 80-120 DEG C. The acetal/ketal is obtained by aftertreatment of the reaction liquid after the reaction is completed. The acidic ionic liquid is a 3-(3-sulfonic acid)propyl benzothiazole salt acidic ionic liquid. The alcohol is C2-C4 organic alcohol. The method for synthesis of acetal/ketal catalyzed by the acidic ionic liquid has the advantages that the reaction operation is simple and convenient; separation of the catalyst from the product is easy; product purity and yield are high; and the catalyst can be reused and the catalytic activity thereof is essentially same. Accordingly, the method has broad application prospects.

The invention relates to a synthetic method of tetra(dimethylamino)hafnium, which comprises the following steps: in an argon atmosphere, adding dimethylamine and n-hexane into a three-necked bottle, evenly mixing, putting the reaction bottle at -40--80 DEG C, dropwisely adding an n-butyllithium solution into the reaction bottle, and mixing to react for 10 hours; adding hafnium tetrachloride into the reaction system, keeping the temperature of the reaction system at 20-60 DEG C, and after finishing adding the hafnium tetrachloride, mixing the reaction system under inert gas shielding to react for 24-30 hours; after the reaction finishes, removing the reaction solvent in one atmosphere; and after all the solvent n-hexane is removed, carrying out reduced pressure distillation to collect 80-85 DEG C/2-5mmHg fraction which is the tetra(dimethylamino)hafnium compound. The dimethylamine, butyllithium and zirconium tetrachloride which are simple and accessible are used as the reaction raw materials; and thus, the invention is simple to operate and lowers the cost.

The invention discloses a continuous synthesizing method of indoor ion liquid, which comprises the following steps: adopting pyridine or N-alkyl imidazole and halogenated hydrocarbon under normal pressure; stirring; making hydrocarbyl pyridine ammonium halides or 1, 3-dialkyl imidazole ammonium halides; adding fluorine salt to stir to react; obtaining the ion liquid under normal temperature; avoiding pollution due to using organic solvent; temperating reacting condition; improving reacting receiving rate and product quality; fitting for large scale of industrial manufacturing.

The invention relates to a method for preparing paraphthaloyl chloride. The method comprises the following steps: mixing thionyl chloride and terephthalic acid according to the mass ratio of 2:1 to 5:1; adding one or more of nitrogen-containing organic bases such as substituted pyrrolidine, substituted piperidine, substituted pyridine, (substituted) quinoline, (substituted) isoquinoline, (substituted) phenanthroline, substituted imidazole, substituted benzimidazole and the like as a catalyst, which are 0.5-2% of mass of terephthalic acid; reacting at 70-120 DEG C for 4-16 hours; distilling and recovering excessive thionyl chloride; distilling or rectifying in vacuum to recover the catalyst, so as to obtain the product paraphthaloyl chloride by vacuum rectification, wherein the yield can be up to 96%, and the purity is higher than 99%. The method has the advantages that the catalyst is low in price and available, and can be recycled, the product is high in yield and purity, the reaction operation is simple and convenient and the like.

The invention provides a preparation method of ilaprazole. According to the method, ilaprazole is prepared through a thioether intermediate; obtained ilaprazole is high in quality and has no overoxidation impurities; the method is simple and easy, high in yield, low in cost, environment-friendly, and suitable for industrial production, and has no need for special equipment; and no toxic chloroform solvent is used.

The invention discloses a polymer containing a cyclic azobenzene-dinaphthalene structure on a side chain as well as a preparation method and application of the polymer. Specifically, the polymer has a structure shown by a formula I, and is prepared by the method comprising the following steps: (1) obtaining two types of donors; (2) connecting the two types of donors and performing closed-loop reaction; (3) synthesizing a cyclic monomer; and (4) synthesizing the polymer. The polymer disclosed by the invention is relatively good in product processability and mechanical property, and relatively narrow in molecular weight distribution; meanwhile, a general free radical polymerization method is adopted to synthesize asymmetrical monomers into a chiral optical polymer, and the experimental operation is simple and feasible, so that a new idea is provided for designing and synthesizing polymer chiral optical switches; and moreover, the chemical reagents used in the method disclosed by the invention are stable in the air, and the method is simple and convenient to operate, is high in efficiency and is convenient for industrial production.

The invention relates to the field of synthesis of compounds, in particular to a new method for synthesizing 6- methyl-17alpha-acetoxyl-19-norpregna-4,6-dialkyl-3,20-diketone. According to the method provided by the invention, norethindrone is taken as starting material to prepare 6- methyl-17alpha-acetoxyl-19-norpregna-4,6-dialkyl-3,20-diketone, the method provided by the invention has the advantages that the defects in the prior art are overcome, operation is simplified and production cost is reduced, related reactions and operations are simple, yield is high, and the yield of each step is 80% or above.

The invention discloses a method for preparing starch sulphate with high degree of substitution. In the method, sulfur trioxide pyridine is taken as an esterifying agent, dimethylformamide is taken as a dissolvent, and the sulfur trioxide pyridine and the dimethylformamide are used for esterfying starch so as to obtain the starch sulphate with high degree of substitution being 0.2-0.9, wherein the mass ratio of the sulfur trioxide pyridine to the starch is (1:1)-(5:1). Solid sulfur trioxide pyridine is taken as a sulfonating agent, so that the method is easy to control, the reaction operation is convenient and the sulfonation reaction degree is higher; in addition, by utilizing the method, corrosion of strong acid liquids on equipment can be avoided; and the dissolvent is convenient to recycle, thus preferably avoiding pollution to environments.

The invention relates to a preparation method of avanafil and a new compound provided in a preparation process. According to the method, 5-uracil carboxylic acid or an ester thereof is taken as the raw material, and the avanafil meeting the clinical requirements can be synthesized at a relatively cost; besides, the preparation method is simple and convenient to operate, mild in reaction conditions, high in yield, low in cost, environmentally friendly and suitable for industrial large-scale production of the avanafil.

The invention discloses a preparation method of a bifunctional MOF (Metal Organic Framework) nano-catalyst for degrading p-nitrophenol and simultaneously fixing nitrogen at room temperature and application of the bifunctional MOF nano-catalyst based on bifunctional electrocatalysis of the catalyst, and belongs to the technical field of metal organic framework material technologies and nano-catalysis. The preparation method comprises the following main steps: blending an isophthalic acid ligand solution with a mixed solution of zinc nitrate and cobalt nitrate, and adding a triethanolamine solution and activated carbon cloth to prepare a carbon cloth loaded Zn-MOF and Co-MOF crystal composite material; and activating the composite material in a 250 W microwave oven for 3 min to obtain the bifunctional MOF nano-catalyst. The catalyst is prepared from low-cost raw materials, is low in reaction energy consumption and has a good industrial prospect. The catalyst is used for degrading p-nitrophenol and fixing nitrogen at room temperature, and has the advantages of simple equipment, high electrochemical stability and the like.