26results about How to "Few reaction steps" patented technology

The application discloses a method for synthesizing tervalent tetraaryl iron porphyrin from pyrrole, aromatic aldehyde and ferrous salt, which comprises the following steps: adding anhydrous aluminum chloride, aromatic aldehyde, pyrrole and ferrous salt into DMF under stirring, and then heating and refluxing the reaction mixture for 0.5 hours under nitrogen; removing the nitrogen and continuing to heat the reaction mixture for a certain time; stopping the reaction; cooling the reaction mixture; and placing the reaction mixture at 273K overnight; and finally filtering the reaction mixture to obtain the iron porphyrin.

The invention discloses a method for preparing phenyl acetate with high selectivity. A phosphoric acid solution is added into a magnesium chloride solution, stirring and heating are performed to obtain a suspension, the suspension is dried to constant weight to obtain a white solid, the white solid is ground to obtain powder, and the powder is calcined to obtain the catalyst. Then mixing phenol and a catalyst, placing the mixture in an oil bath for reflux reaction, dropwise adding acetic anhydride, distilling after the reaction is finished, and collecting a fraction at 190-195 DEG C, namely phenyl acetate. According to the magnesium chloride loaded phosphoric acid type catalyst (MgCl2-H3PO4) prepared by the method disclosed by the invention, phenol and acetic anhydride react without a solvent, MgCl2-H3PO4 is a solid catalyst, can be recycled only by filtering and can be repeatedly used after being washed, and MgCl2-H3PO4 also improves the selectivity of phenyl acetate and reduces the production cost.

This invention provides a method for preparing 4,1-disubstituted pyrrolo[1,2-a]quinoxaline-1-yl ketone derivatives, belonging to the field of organic synthesis technology. This invention uses 2-(1H-pyrrolo-1-yl)aniline compounds and α-carbonyl acids as reactants, employing only ammonium persulfate as an oxidant. Under metal-free catalysis, a one-pot tandem reaction is carried out to simultaneously complete the cyclization of the pyrrolo[1,2-a]quinoxaline nucleus and the C-1 acylation modification. The substituents at the 4- and 1-positions of the product can be flexibly controlled by changing the α-carbonyl acid with different structures. This method requires no pre-modified substrate, eliminates the need for metal catalysts, avoids the risk of metal residue, and features simplified steps and high functional group compatibility, providing a new green and low-cost route for the synthesis of polysubstituted pyrrolo[1,2-a]quinoxaline ketone derivatives.

The application discloses a preparation method of a trans-7H-pyrrolo[2,3-d]pyrimidine compound, and the full name of the trans-7H-pyrrolo[2,3-d]pyrimidine compound is trans-N-methyl-4-(methyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)cyclohexylmethanesulfonamide maleate, which is prepared from trans-4-[(tert-butoxycarbonyl)amino]cyclohexane carboxylic acid and 4-chloro-7H-pyrrolo[2,3-d]pyrimidine as starting materials through reduction, chlorination, substitution, oxidation, methylation, condensation and salt formation reactions. The preparation method has the advantages of few reaction steps, simple operation, low production cost, high production efficiency, high yield, high product purity and suitability for scale-up production.

The invention discloses photocatalytic stereoselective E-type olefination of alkynyl amide and a preparation method of the alkynyl amide. The method is carried out in a water-phase micelle reaction system and is completed under the driving of visible light. According to the method, an alkynyl amide compound is taken as a raw material, sodium ascorbate is taken as a green reducing agent, Ru (bpy) 3 (PF6) 2 or [Ir (dtbpy) (ppy) 2] PF6 is taken as a photocatalyst in a water-phase micelle environment formed by a surfactant lauryl sodium sulfate (SDS), and under the protection of inert gas, catalytic circulation is initiated by visible light irradiation at 20-40 DEG C, so that the alkynyl amide compound is highly selectively converted into an E-type olefin product. The method is mild in condition, simple in step, high in stereoselectivity, environment-friendly and safe to operate, the problem that flammable and explosive reagents or harsh reaction conditions need to be used in a traditional method is solved, and a green and efficient preparation way is provided for preparation of the E-type acrylamide compound.

The invention relates to the technical field of medical instruments, in particular to a heparin coating based on material surface ammonification modification and a preparation method thereof, and the preparation method at least comprises the following steps: carrying out ultrasonic pretreatment on a base material with purified water, and drying for later use; the preparation method comprises the following steps: performing amination modification on a base material subjected to ultrasonic pretreatment by adopting an ammoniation reagent solution, and immersing the base material into a heparin solution to prepare the base material with a heparin coating on the surface. The surface of the material is subjected to amination modification by adopting a micromolecular ammoniation reagent and / or a macromolecular ammoniation reagent system, complex pretreatment such as plasma and ultraviolet rays does not need to be carried out on a base material, specific functional group activation does not need to be carried out on heparin, and the heparin is directly reacted after being subjected to ammoniation modification; the stable covalent grafted heparin anticoagulation coating can be formed, the anticoagulation time is prolonged, and the long-term implantation requirement is met.

This invention discloses a highly efficient oxygen removal reagent and its application in the deoxygenation reconstruction of carbon resource molecular skeletons, comprising a pivot reagent, a phosphine reagent, an azo reagent, a reducing agent, an acid reagent, a base reagent, a photosensitizer, and an organic solvent; wherein, X in the pivot reagent includes a hydrazine group or a sulfone group; PG is a protecting group; LG is a leaving group; by using natural oxygen-containing functional groups such as alcohols, aldehydes, and ketones as direct coupling precursors, an integrated in-situ activation-deoxygenation coupling process is achieved, significantly reducing reaction steps.

This invention discloses a deuterated scintillator with a space charge transfer structure, its preparation method, and its application in X-ray scintillation imaging, belonging to the field of scintillator materials. The scintillator structure of this invention is characterized by using tripterene as a bridging unit to connect a planar nitrogen-oxygen donor and a deuterated boron-oxygen acceptor. While ensuring high X-ray absorption capacity, it reduces the non-radiative transition rate, achieving a synergistic effect of high luminescence quantum yield, fast decay lifetime, and low self-absorption, thus meeting the requirements of high-resolution, high-sensitivity X-ray imaging. A transparent and highly flexible organic gel scintillator film is prepared by blending and polymerizing an X-ray-responsive organic scintillator with hydroxyethyl methacrylate. This film exhibits highly efficient luminescence under both photoluminescence and radiative luminescence conditions, significantly improving X-ray imaging sensitivity and resolution. Experiments show that the organic gel scintillator film prepared by this invention achieves a resolution of over 16.0 lp / mm under standard line-pair cards.

The present application relates to a preparation method of CL2A-SN-38, the preparation method comprises the following steps: (1) reaction of intermediate 3 and compound 2 to prepare intermediate 4; (2) dehydroxy protection group and then deamination protection group of intermediate 4 prepared in step (1) to prepare the CL2A-SN-38. The preparation method of CL2A-SN-38 has the advantages of few reaction steps, simple operation, low cost, high purity and yield, and is suitable for industrial production.

The application discloses a preparation method of S4-(2-cyanoethyl)-4-thiothymine deoxyriboside monomer, and 5'-O-DMT-uridine is used as a starting material. First, the starting material is reacted with a sulfonylation reagent to generate a sulfonylation reaction on a carbonyl group at a 4 position of the starting material to obtain compound II. Then, the compound II is reacted with 3-mercapto propionitrile to continuously generate a substitution reaction on the 4 position to obtain compound III. Finally, the compound III is reacted with a phosphorus reagent to obtain the S4-(2-cyanoethyl)-4-thiothymine deoxyriboside monomer. The method does not need to protect a 3'-hydroxyl group, has a shorter reaction route, milder reaction conditions, and high synthesis efficiency.

This invention relates to the field of new energy materials technology, and discloses a self-assembled molecular material and its applications. The self-assembled molecular material has the structure shown in Formula I: Formula I; wherein A is a substituted or unsubstituted carbazole group, B is a substituted or unsubstituted fluorene group, A' is a substituted or unsubstituted carbazole group or a substituted or unsubstituted triphenylamine group; and D is an anchoring group. This self-assembled molecular material simultaneously includes a fluorene structure, a carbazole structure, and multiple anchoring groups. The synergistic interaction of these groups and structures significantly enhances the thermal stability and film-forming properties of the self-assembled molecular material, resulting in solar cells containing this self-assembled molecular material exhibiting excellent photothermal conversion efficiency and stability.

The invention discloses a preparation method of 4 '; the novel preparation process comprises the following steps: under the protection of inert gas, dissolving a chiral ligand and a metal salt in an organic solvent, stirring the mixture for 30 minutes to 1 hour at room temperature, adding a solution of a compound II into a catalyst solution, stirring for 15-30 minutes at a low temperature of-40 DEG C, adding a compound I, an activating agent and an alkali reagent, stirring for 15-30 minutes at a low temperature of-40 DEG C, and reacting for 1-2 hours to obtain a compound I; and continuously stirring at-40 DEG C to react for 6-8 hours, monitoring the proceeding of the reaction by HPLC (High Performance Liquid Chromatography), and separating a product after the reaction is completed to obtain a compound III. The method has the beneficial effects that the operation is simple, the reaction steps can be effectively reduced, the reaction route is short, the raw materials are easy to obtain, the reaction time is short, and the production cost and the labor cost can be effectively reduced; the product yield is high, the reaction selectivity is good, the product purity is high, the reaction product yield is high, the selectivity is good, the target product can be obtained at a high yield, and meanwhile, the post-treatment difficulty of the product is reduced.

This invention discloses a method for synthesizing pyrrole compounds using solid acid catalysis. The method is as follows: in the presence of a carbon-based solid acid catalyst, β-nitrostyrene compounds represented by formula (1), acetyl acetate represented by formula (2), and primary amine represented by formula (3) are reacted in a solvent in a one-pot reaction. After the reaction is completed, the reaction solution is post-treated to obtain polysubstituted pyrrole compounds represented by formula (4). In the preparation of polysubstituted pyrrole compounds by this invention, the reaction can proceed smoothly under carbon-based solid acid catalysis without the need for other additives, making it safe, environmentally friendly, and with mild reaction conditions. The reaction formulas are as follows: in formulas (1) to (4), substituent R1 is H, C1-C5 straight-chain or branched alkyl or alkoxy, halogen, nitro, etc.; substituent R2 is C1-C10 straight-chain or branched alkyl, C5-C6 cycloalkyl, benzyl, etc.; substituent R3 is selected from C1-C5 straight-chain or branched alkyl, phenyl, benzyl, or substituted benzyl.

The oxazole ring, as a classical nitrogen-containing heteroaromatic ring skeleton, has irreplaceable application value in the frontier fields of pharmaceutical chemistry, functional material creation, bioactive molecule research and development and the like. Wherein the methyl oxazole-2-formate has become a core synthesis precursor of a variety of pharmaceutical molecules and high value-added fine chemicals by virtue of unique structural characteristics and reaction activity. In order to solve the common bottleneck problems of low yield, insufficient product purity, strict reaction conditions and the like in the existing synthesis process, the invention aims at efficient and green synthesis of oxazole-2-methyl formate, and systematically explores the regulation and control effects of key parameters such as reaction solvent, reaction time, reaction temperature, type and dosage of alkali and the like on the synthesis process. Results show that 1.0 equivalent of 1H-1, 2, 3-triazole and 1.2 equivalent of oxalyl chloride monomethyl ester are taken as initial raw materials, 1.0 equivalent of sodium hydride and 1.0 equivalent of potassium carbonate are adopted to construct a mixed base catalysis system, sulfolane is taken as a solvent, reaction is performed for 2 hours at the temperature of 80 DEG C, the oxazole-2-methyl formate can be efficiently prepared through a one-pot method, the product yield reaches up to 92%, and the purity reaches up to 98%. The purity of the product obtained by the process meets the application requirements of subsequent separation and purification of medical intermediates, structural modification and large-scale preparation, a feasible technical path is provided for industrial production of oxazole derivatives, and the method has remarkable application potential and popularization value.

The application splits the molecular structures of phenylpyrimidine and benzamide, and discloses aniline pyrimidine compounds by means of computer-aided drug design. Research results show that the aniline pyrimidine compounds have PLK1 inhibitory activity and have obvious inhibitory effect on cancer cells. The application also provides a preparation method of the aniline pyrimidine compounds. The method is scientific and reasonable, simple and easy to operate, has few reaction steps, high yield and is suitable for industrial production.

The invention belongs to the technical field of mineral processing and beneficiation reagents, and particularly relates to a double-phenyl-bridged dihydroximic acid flotation collecting agent and a preparation method and application of the double-phenyl-bridged dihydroximic acid flotation collecting agent. The general chemical formula of the biphenyl bridged dihydroximic acid flotation collecting agent is HO-NHC (= O)-Ar-O-R-O-Ar-C (= O)-NHOH; wherein Ar is an aromatic ring group of which the ortho-position is provided with carboxyl or carboxylic ester group; and R is alkylene with 1-8 carbon atoms. The collecting agent with the double-benzene-ring double-hydroximic-acid structure is expected to have higher selectivity, more stable chelation capacity and higher hydrophobicity at the same time, so that the collecting agent shows excellent collecting effect and separation efficiency in the flotation process, and the defects that an existing hydroximic acid agent is insufficient in selectivity, poor in hydrophobicity and the like are effectively overcome.

The invention discloses a synthesis method of beta alkylamine, and belongs to the field of organic synthesis. According to the method, 3-phenyl-1, 4, 2-dioxazole-5-ketone and 1, 1-disubstituted alkyl olefin are subjected to a mixed coupling reaction in an organic solvent system in the presence of a transition metal catalyst, a nitrogen ligand, a reducing agent, alkali and an additive to synthesize the beta-alkylamine. Cheap cobalt metal is used as a catalyst, a coupling reaction of beta-alkylamine is constructed, and the method has the advantages of mild reaction conditions, high economical efficiency and the like.

The invention discloses a preparation method of a chiral amine derivative with a far-end boric acid ester functional group, and develops a method for obtaining a chiral amine compound containing the far-end boric acid ester functional group by one-step construction and separation through a transition metal catalyzed boron amination method by taking an aldehyde compound which is easy to prepare as an initial raw material. Various functional groups are converted through a simple chemical reaction, and the cyclic or non-cyclic chiral amine compound containing various functional groups is prepared. The synthesis method provided by the invention has the advantages of easiness in preparation of raw materials, high atom economy, easiness in separation, wide application and the like.

The invention belongs to the technical field of chemical synthesis of medicines, and particularly relates to a synthesis method of an LXH-1211 intermediate. The preparation method comprises the following steps: carrying out stirring reaction on phenylhydrazine, 3-aminocrotonitrile and a reaction solvent to obtain an intermediate IM-1; mixing the intermediate IM-1 and a reaction solvent, cooling, adding phosphorus oxychloride, and heating for reaction to obtain an intermediate IM-2; and dissolving the intermediate IM-2 in a reaction solvent, adding ethyl cyanoacetate, and carrying out a stirring reaction to obtain the LXH-1211 intermediate. The raw materials are easy to obtain, use of highly toxic and explosive materials, column chromatography and other operations are avoided, the yield is remarkably improved, special equipment is not needed, industrial amplification is facilitated, and the environmental protection cost is effectively reduced.

The present application belongs to the technical field of preparation of alpha-branched alkenone, and particularly relates to a preparation method of beta-amino substituted alpha-branched alkenone compound. The present application uses beta-acyl allyl sulfide, amine compound and silver carbonate as reaction raw materials, controls reaction temperature and time in a solvent to synthesize the beta-amino substituted alpha-branched alkenone compound. The synthesis method used in the present application can realize the preparation of beta-amino substituted alpha-branched alkenone in only one step. Compared with traditional synthesis reaction, the synthesis method expands the substrate range, shortens the reaction steps, improves the total synthesis yield, reduces the reaction cost, and provides a more economical, efficient and practical synthesis new route for the synthesis of beta-amino substituted alpha-branched alkenone.

The invention provides a preparation method of buracametacin, which comprises the following steps: dissolving tetrahydro-N, N-dimethyl-5-oxo-2, 2-diphenyl-3-furanformamide with tetrahydrofuran, adding sodium borohydride and a boron trifluoride diethyl etherate complex, and carrying out reflux reaction to obtain the buracametacin.

The invention discloses a chiral bridged metallocene compound as well as a preparation method and application thereof, and the chiral bridged metallocene compound is characterized in that the chiral bridged metallocene compound has a general formula (I): wherein R1 is selected from 4-substituted phenyl; r2 is selected from alkyl; m is selected from one of Ti, Zr and Hf; x is selected from halogen. The catalyst prepared from the chiral bridged metallocene compound has better catalytic activity, the melt index and isotacticity of synthesized polypropylene are improved, and a polypropylene material with better fluidity can be obtained.

The invention belongs to the technical field of organic synthesis, and particularly relates to an aryl formyl pyrazole compound and a synthesis method thereof. The synthesis method comprises the following steps: uniformly dispersing an aryl formic acid compound as shown in a formula 1 and a pyrazole alcohol compound as shown in a formula 2 in an organic solvent, stirring at room temperature, and sequentially adding an organic alkali and an onium salt condensing agent, so that the aryl formyl pyrazole compound can be efficiently prepared, the yield of the target compound is as high as 93%, and the aryl formyl pyrazole compound can be prepared by modifying hydroxyl on a pyrazole ring. A prodrug of the drug molecule or a compound with potential biological activity is obtained; according to the method disclosed by the invention, esterification and rearrangement two-step reaction are completed by a one-pot method under a one-step condensation condition for the first time, reaction steps are effectively shortened, and the preparation cost is remarkably reduced while the atom economy is greatly improved. Meanwhile, the method effectively overcomes the harsh reaction conditions of using highly toxic pipe products such as acetone cyanohydrin and trimethylsilyl cyanide in the existing rearrangement technology, and overcomes the technical defects of complex substrate synthesis, limited range and the like.

The application belongs to the technical field of medicine synthesis, and particularly relates to a butenafine intermediate compound and a preparation method thereof. The butenafine intermediate compound I is prepared by taking N-(4-tert-butylbenzyl)-naphthalenemethylamine as a starting material, and reacting the starting material with an acylation reagent under the action of an acid binding agent. The hydrochloric acid butenafine is prepared by performing a one-step reduction reaction on the compound I. Compared with the prior art, the preparation method can effectively avoid the use of genotoxic reagents, such as methyl iodide and formaldehyde. The target product is obtained by performing a one-step salification on a crude product, so that the reaction steps are less, the post-treatment is simple, the yield and purity are relatively high, and the method is more suitable for industrial production.

This invention belongs to the technical field of flame-retardant polyether polyols and their preparation, specifically relating to a method for preparing a highly flame-retardant phosphazene-based polyether polyol. The method involves a nucleophilic substitution reaction between hexachlorocyclotriphosphazene and water in the presence of an acid-binding agent, generating a polyhydroxyl-containing phosphazene derivative as an initiator. Using this initiator as the core, other small-molecule polyols are combined, and propylene oxide undergoes ring-opening polymerization under the action of a catalyst to form a polyether polyol with a "phosphazene ring-polyether chain" structure. Due to the presence of the phosphazene ring in the molecule, this product possesses both excellent flame-retardant properties and good reactivity, and can be directly used to synthesize flame-retardant rigid polyurethane foams, elastomers, and other materials, solving the problem of requiring additional flame retardants in traditional polyether polyols. This invention features highly controllable processes, readily available raw materials, and a product with excellent comprehensive performance, making it highly valuable for industrial applications.

The present disclosure provides a method for preparing and purifying 4-dihydroxyboryl-L-phenylalanine, comprising reacting 4-halo-phenylalanine with a Grignard reagent in the presence of an amidine compound or a guanidine compound without using a protecting group for an amino group of the 4-halo-phenylalanine, thereby reducing reaction steps and improving reaction efficiency.