21 results about "Phosphorus tribromide" patented technology

The application discloses a preparation method of a key intermediate of a montelukast sodium side chain acid, belongs to the technical field of pharmaceutical intermediates, and relates to a key intermediate of a montelukast sodium side chain acid, i.e. 1-bromomethylcyclopropylacetonitrile, which is characterized by the preparation method of the 1-bromomethylcyclopropylacetonitrile. The preparation method is as follows: taking tribromoneopentyl alcohol as a starting material, and obtaining 1-bromomethylcyclopropylacetonitrile through a cyclization reaction, an iodination reaction and a cyano substitution reaction. The 1-bromomethylcyclopropylacetonitrile is prepared by using a brand-new synthesis process, starting from tribromoneopentyl alcohol, through a cyclization reaction, an iodination reaction and a cyano substitution reaction. The method solves the blank of the preparation method of 1-bromomethylcyclopropylacetonitrile in the prior art, and also solves the defects of a long reaction theoretical cycle and a low actual yield and a large amount of impurities in the reaction of preparing 1-bromomethylcyclopropylacetonitrile by first preparing 1-hydroxymethylcyclopropylacetonitrile and then reacting phosphorus tribromide with the 1-hydroxymethylcyclopropylacetonitrile.

This invention belongs to the field of pharmaceutical synthesis technology, specifically relating to a synthetic process for tetraacetyl gastrodin. It involves first preparing tetraacetyl glucose bromide using phosphorus tribromide, then reacting the tetraacetyl glucose bromide with a sodium alkoxide to obtain a condensation product, which is then reduced to yield tetraacetyl gastrodin. Therefore, under anhydrous conditions, the brominated sugar does not undergo hydrolysis, avoiding the loss of the brominated sugar raw material and thus improving the yield.

The application belongs to the technical field of fine chemical industry, and particularly relates to a hydrogen bromide purification method for removing bromine, water and impurities before liquefaction, which comprises the following steps: S1, removal of free bromine: hydrogen bromide gas is introduced into a first bromine removal tank filled with a red phosphorus filler layer; S2, preliminary removal of water: the gas treated in S1 is introduced into a first drying tank filled with liquid phosphorus tribromide; S3, deep removal of trace water: the gas treated in S2 is introduced into a second drying tank filled with resin or mordenite; and S4, separation of mechanical impurities: the gas treated in S3 is introduced into a cyclone separator. By adopting the red phosphorus filler layer and controlling the loading amount, particle size and loading density of the red phosphorus, the free bromine in the hydrogen bromide gas can be efficiently removed, liquid phosphorus tribromide is used as a drying medium and is supplemented in real time to maintain the mass concentration of the phosphorus tribromide, so that the bromine and water content in the gas can be effectively reduced, and high-quality gas is provided for subsequent deep drying and impurity separation.

The invention discloses a chemical intermediate phosphorus oxybromide preparation method, which comprises: S1, mixing phosphorus tribromide and [BMIM] Br, and stirring at a temperature of 30-50 DEG C to obtain a mixture I; s2, adding red phosphorus into the mixture 1, and pre-dispersing in a supercritical CO2 medium to obtain a mixture II; s3, stage I: introducing bromine into the mixture II at the temperature of-5 to 0 DEG C, synchronously dropwise adding tetrabutylammonium bromide and crown ether, and maintaining the pH value of the system to be 1.5-2.0; stage II: raising the temperature to 33-37 DEG C; and stage III: raising the temperature to 40-60 DEG C to obtain a crude product of phosphorus oxybromide. According to the invention, the following breakthrough progress is realized through innovative process design: a high-efficiency atom economy synthesis path is combined with a supercritical medium dispersion technology through an ionic liquid concerted catalysis system, so that the bromine reaction activity and the mass transfer efficiency are remarkably improved; the problems of excessive addition of raw materials and large generation amount of byproducts in the traditional process are fundamentally solved, and efficient utilization of bromine resources is realized.

The invention discloses a binuclear piperidine ionic liquid and a preparation method thereof. The dinuclear piperidine ionic liquid is prepared by taking glycol, phosphorus tribromide, piperidine, alkyl sultone and a sulfonic acid derivative as raw materials. The method comprises the following steps: preparing dibromoglycol by taking glycol and phosphorus tribromide as raw materials; piperidine and dibromoethylene glycol react to prepare a binuclear piperidine intermediate; reacting the binuclear piperidine intermediate with alkyl sultone to prepare binuclear piperidine sulfonic acid inner salt; the binuclear piperidine ionic liquid is prepared by taking binuclear piperidine sulfonic acid inner salt and a sulfonic acid derivative as raw materials. The invention provides a new scheme for preparing the polyfunctional group piperidine ionic liquid.

The invention belongs to the field of new energy materials, and particularly relates to a viologen electrolyte with multi-electron transfer capability, a preparation method and application of the viologen electrolyte in an aqueous organic flow battery. The preparation method comprises the following steps: reacting triethanolamine with phosphorus tribromide to generate a tris (2-bromoethyl) amine intermediate, condensing the tris (2-bromoethyl) amine intermediate with 4, 4 '-dipyridyl to generate a trinuclear viologen precursor, and finally performing quaternization and anion exchange to obtain a target product. The solubility of the prepared viologen electrolyte in an aqueous solution reaches up to 1.82 M, the theoretical charge capacity is 103 Ah L <-1 >, and the viologen electrolyte can perform highly reversible multi-electron redox reaction and shows excellent electrochemical performance. When the material is applied to the aqueous organic flow battery as a negative electrode active material, the battery shows the outstanding advantages of high coulombic efficiency, high energy density, long cycle life and the like.

The invention discloses a synthesis method of octadecanedioic acid, and belongs to the field of chemical synthesis. The method comprises the following steps: adding phosphorus tribromide and acetonitrile into a three-neck bottle, and heating in a nitrogen atmosphere; then slowly dropwise adding a mixed solution of 1, 12-dodecanediol and DMF (Dimethyl Formamide), and after dropwise adding is completed, heating the reaction solution again and reacting; and cooling the reaction liquid, dropwise adding water, extracting with petroleum ether, washing a petroleum ether layer with a saturated saline solution, adding anhydrous sodium sulfate into the petroleum ether layer, and drying, filtering and concentrating to obtain a faint yellow solid. By constructing a molecular skeleton step by step, accurate regulation and control of an intermediate are realized, and complex side reactions are avoided. According to the method, mild reaction conditions are adopted, special requirements on equipment are effectively reduced, and meanwhile, energy consumption is reduced. In the aspect of raw material selection, expensive or highly toxic substances are replaced with commercialized reagents easy to obtain, and cost controllability and environment friendliness are both considered.

The present invention discloses a type I photosensitizer and its preparation method and application. The preparation method of the photosensitizer comprises the following steps: (1) 780 The method comprises reacting 5-bromobenzene-1,3-diol with 5-bromobenzene-1,3-diol in the presence of an acid-binding agent and a solvent to obtain compound CyBr; reacting Fmoc-L-alanine with p-aminobenzyl alcohol in the presence of a condensing agent, a catalyst, and a solvent to obtain intermediate 2; reacting intermediate 2 with phosphorus tribromide in the presence of a solvent to obtain intermediate 3; (2) reacting compound CyBr with intermediate 3 in the presence of an alkaline reagent, a catalyst, and a solvent to obtain intermediate 4; and reacting intermediate 4 with piperidine in the presence of a solvent to obtain the type I photosensitizer. The type I photosensitizer can specifically target the biomarker aminopeptidase highly expressed in tumors, achieve precise tumor imaging and photodynamic therapy, and after light excitation, can serve as a stimulus source to stimulate the body's immunity, initiate anti-tumor immunity, eliminate primary residual tumors, and inhibit distant metastatic tumors.

The application discloses a benzoxazine compound and a preparation method thereof, and belongs to the field of chemical industry.The preparation method comprises the following steps: (1) condensation reaction of compound S01 and compound S02 in a first reaction solvent under the action of a condensation agent, wherein the reaction temperature is 0-40 DEG C, the reaction time is 3-24 h, and the compound M1 is obtained through cooling, concentration and recrystallization; (2) substitution reaction of the compound M1 and phosphorus tribromide in a second reaction solvent, wherein the reaction temperature is 0-50 DEG C, the reaction time is 3-24 h, and the compound M2 is obtained through cooling, concentration and recrystallization; (3) condensation reaction of the compound M2 and paraformaldehyde in a third reaction solvent under the action of an acid, wherein the reaction temperature is 0-100 DEG C, the reaction time is 3-24 h, and the compound M3 is obtained through cooling, concentration and recrystallization; and (4) reaction of the compound M3 and compound S03 in a fourth reaction solvent, wherein the reaction temperature is 0-120 DEG C, the reaction time is 8-24 h, and the target compound is obtained through cooling, concentration and recrystallization. The application has high, broad and persistent bactericidal effect, and has wide application prospect and development space.

This invention discloses a method for synthesizing bifonazole, belonging to the field of pharmaceutical synthesis technology. The method uses 4-phenyldibenzyl alcohol and imidazole as raw materials, and phosphorus tribromide, phosphorus trichloride, or phosphorus oxychloride as condensing agents, to directly condense bifonazole in a solvent. The reaction conditions are mild, can be carried out at room temperature, the reaction is complete with few impurities, and the yield is high; it has low equipment requirements and is suitable for large-scale production.

The invention discloses polyfunctional group four-season ammonium ionic liquid and a preparation method thereof. According to the invention, 1, 4-diazido-bicyclo [2, 2, 2] octane, glycol, phosphorus trichloride or phosphorus tribromide, alkyl sultone and a sulfonic acid derivative are used as raw materials to prepare the polyfunctional group four-season ammonium ionic liquid; the method comprises the following steps: preparing dibromo (chloro) glycol by taking glycol, phosphorus trichloride or phosphorus tribromide as raw materials; the preparation method comprises the following steps: reacting 1, 4-diazido-bicyclo [2, 2, 2] octane with dibromo (chloro) glycol to prepare a tetranuclear quaternary ammonium intermediate; reacting the tetranuclear quaternary ammonium intermediate with alkyl sultone to prepare tetranuclear quaternary ammonium sulfonic acid inner salt; the polyfunctional group four-season ammonium ionic liquid is prepared by taking tetranuclear quaternary ammonium sulfonic acid inner salt and a sulfonic acid derivative as raw materials. The invention provides a new scheme for preparing the multifunctional ionic liquid.

The invention discloses a multifunctional binuclear morpholine ionic liquid and a preparation method thereof. According to the invention, glycol, phosphorus trichloride or phosphorus tribromide, morpholine, alkyl sultone and a sulfonic acid derivative are used as raw materials to prepare the multifunctional binuclear morpholine ionic liquid. The method comprises the following steps: preparing dibromo (chloro) glycol by taking glycol, phosphorus trichloride or phosphorus tribromide as a raw material; the preparation method comprises the following steps: reacting morpholine with dibromo (chloro) glycol to prepare a binuclear morpholine intermediate; reacting the binuclear morpholine intermediate with alkyl sultone to prepare binuclear morpholine sulfonic acid inner salt; the polyfunctional group binuclear morpholine ionic liquid is prepared by taking binuclear morpholine sulfonic acid inner salt and a sulfonic acid derivative as raw materials. The invention provides a new scheme for preparing the multi-functional group morpholine ionic liquid.

The invention discloses polyfunctional group pyrrole acidic ionic liquid and a preparation method thereof. The polyfunctional group pyrrole acidic ionic liquid is prepared by taking glycol, phosphorus trichloride or phosphorus tribromide, pyrrole, alkyl sultone and a sulfonic acid derivative as raw materials. The method comprises the following steps: preparing dibromo (chloro) glycol by taking glycol, phosphorus trichloride or phosphorus tribromide as a raw material; the preparation method comprises the following steps: reacting pyrrole with dibromo (chloro) glycol to prepare a dinuclear pyrrole intermediate; reacting the dinuclear pyrrole intermediate with alkyl sultone to prepare dinuclear pyrrole sulfonic acid inner salt; the polyfunctional group pyrrole acidic ionic liquid is prepared by taking dinuclear pyrrole sulfonic acid inner salt and a sulfonic acid derivative as raw materials. The invention provides a new scheme for preparing the polyfunctional group acidic ionic liquid.

The application discloses a preparation method of Roxadustat, which comprises the following steps: firstly, condensing compound 1 with a condensing agent under the action of an organic base to obtain a hydroxyl acylation intermediate; and secondly, directly coupling the hydroxyl acylation intermediate with methyl boronic acid under the catalysis of a catalyst to obtain a key intermediate compound 2. The improvement avoids the use of phosphorus oxychloride or phosphorus tribromide, effectively reduces the generation of three wastes, shortens the reaction steps, and improves the reaction yield. In the condensation step with a glycine segment, glycine sodium is used to replace glycine, and the amidation reaction of the glycine sodium with the intermediate compound 2 is studied to obtain the final product roxadustat 3. The improvement also greatly reduces the alkaline decomposition by-product of the intermediate compound 2, improves the reaction yield and the purity of the finished product.

Embodiments of the present disclosure generally relate to the field of semiconductor manufacturing processes, more particularly, to precursor chemistries and methods of depositing silicon-containing films for forming semiconductor devices. In one or more embodiments, a method includes co-flowing a silicon-containing precursor with a dopant precursor into a processing chamber at a temperature of 600° C. or less to deposit an epitaxial layer over a substrate disposed within the processing chamber. The silicon-containing precursor is selected from a list consisting of silane (SiH4), disilane (Si2H6), trisilane(Si3H8), tetrasilane (Si4H10), monochlorotrisilane (Si3H7Cl), diiodosilane (SiH2I2), and dibromosilane (SiH2Br2). The dopant precursor selected from a list consisting of phosphine (PH3), phosphorus trichloride (PCl3), phosphorus tribromide (PBr3), tert-butylphosphine (TBP), tri-tert-butylborane ((tBu)3B), tert-butylarsine (TBAs), arsenic trichloride (AsCl3), trisilylphosphine (TSP), triisopropylborane (iPr)3B, tert-butylsilane ((tBu)SiH3), isopropylsilane ((iPr)SiH3), tetrakis(tert-butyl)tin ((tBu)4Sn), tetrakis(isopropyl)tin ((iPr)4Sn), tetrakis(tert-butyl)germane ((tBu)4Ge), tetrakis(isopropyl)germane ((iPr)4Ge), germanium tetrachloride (GeCl4), carbon tetrachloride (CCl4), and hexachlorodisilane (Si2Cl6).

Embodiments of the present disclosure generally relate to the field of semiconductor manufacturing processes, more particularly, to precursor chemistries and methods of depositing silicon-containing films for forming semiconductor devices. In one or more embodiments, a method includes co-flowing a silicon-containing precursor with a dopant precursor into a processing chamber at a temperature of 600 °C or less to deposit an epitaxial layer over a substrate disposed within the processing chamber. The silicon-containing precursor is selected from a list consisting of silane (SiH4), disilane (Si2H6), trisilane(Si3H8), tetrasilane (Si4H10), monochlorotrisilane (Si3H7CI), diiodosilane (SiH2l2), and dibromosilane (SiH2Br2). The dopant precursor selected from a list consisting of phosphine (PH3), phosphorus trichloride (PCI3), phosphorus tribromide (PBr3), tert-butylphosphine (TBP), tri-tert-butylborane ((tBu)3B), tert-butylarsine (TBAs), arsenic trichloride (AsCI3), trisilylphosphine (TSP), triisopropylborane (iPr)3B, tert-butylsilane ((tBu)SiH3), isopropylsilane ((iPr)SiH3), tetrakis(tert-butyl)tin ((tBu)4Sn), tetrakis(isopropyl)tin ((iPr)4Sn), tetrakis(tert-butyl)germane ((tBu)4Ge), tetrakis(isopropyl)germane ((iPr)4Ge), germanium tetrachloride (GeCI4), carbon tetrachloride (CCI4), and hexachlorodisilane (Si2CI6).

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a hydrogen bromide purification method for removing bromine, water and impurities before liquefaction, which comprises the following steps: S1, removal of free bromine: introducing hydrogen bromide gas into a primary bromine removal tank filled with a red phosphorus filler layer; s2, preliminary removal of moisture: introducing the gas treated in S1 into a first-stage drying tank filled with liquid phosphorus tribromide; s3, deep removal of trace water: introducing the gas treated in S2 into a secondary drying tank filled with resin or mordenite; and S4, separation of mechanical impurities: introducing the gas treated in S3 into a cyclone separator. By adopting the red phosphorus filler layer and controlling the filling amount, the particle size and the filling density of red phosphorus, free bromine in hydrogen bromide gas can be efficiently removed, liquid phosphorus tribromide is used as a drying medium and supplemented in real time to maintain the mass concentration of phosphorus tribromide, so that the bromine and moisture content in the gas can be effectively reduced, and the quality of the hydrogen bromide gas is improved. And high-quality gas is provided for subsequent deep drying and impurity separation.

The invention relates to the technical field of imaging coatings, and discloses an imaging coating based on a transparent display screen and a preparation method thereof.The imaging coating of the transparent display screen is obtained by adding modified bentonite, acrylic resin and a radiation absorbent into a stirrer and stirring uniformly; the preparation method comprises the following steps: reacting bentonite with KH560 to obtain epoxy modified bentonite; the preparation method comprises the following steps: reacting cardanol with 2, 2-bis (bromomethyl)-1, 3-propylene glycol to obtain an intermediate A, enabling the cardanol to form disubstitution on the 2, 2-bis (bromomethyl)-1, 3-propylene glycol, and continuously reacting the intermediate A with phosphorus tribromide to obtain bromine modified cardanol; the epoxy modified bentonite, the bromine modified cardanol, polyhedral oligomeric silsesquioxane and ethylenediamine are subjected to a reaction, and modified bentonite is obtained; long chains in the modified bentonite cardanol can be wound with bentonite and polyhedral oligomeric silsesquioxane to form network interpenetration, so that the mechanical properties of the bentonite and the polyhedral oligomeric silsesquioxane are improved, and the mechanical strength of the imaging coating is improved.

This invention belongs to the field of chemical intermediate synthesis technology, specifically relating to a system and method for the continuous preparation of phosphorus oxybromide. The system provided by this invention is designed for continuous production, enabling continuous production of phosphorus oxybromide, improving preparation efficiency, and avoiding the problem of decreased product yield and purity caused by prolonged high-temperature separation. This invention uses phosphorus tribromide as raw material and chloroform as solvent. The mixture is then fed into a reaction tower, where it comes into contact with a mixture of nitrogen dioxide and oxygen entering the tower. Phosphorus tribromide is oxidized to phosphorus oxybromide. Nitrogen dioxide and residual oxygen are recovered and recycled from the top of the reaction tower, reducing waste gas emissions. The mixture of chloroform and phosphorus oxybromide first evaporates most of the solvent in a falling film evaporator, and then evaporates the remaining solvent in a scraped film evaporator, recovering and recycling the solvent. This reduces energy consumption and shortens the time phosphorus oxybromide remains in the evaporator, improving the yield and purity of phosphorus oxybromide.

The invention discloses a colorimetric-fluorescent dual-channel near-infrared probe for H2S specific detection, and a preparation method and application thereof, and belongs to the field of chemical analysis and detection. The preparation method comprises the following steps: firstly, preparing a compound 1 by taking anhydrous N, N-dimethylformamide, dichloromethane, phosphorus tribromide and cyclohexanone as reaction raw materials; reacting the compound 1, cesium carbonate and 2-hydroxy-4-methoxybenzaldehyde to prepare a compound 2; secondly, dropwise adding boron tribromide into a dichloromethane solution in which the compound 2 is dissolved, and reacting to obtain a compound 3; the preparation method comprises the following steps: enabling 3-hydroxy-3-methyl-2-butanone, malononitrile and sodium ethoxide to react to obtain TCF; thirdly, the compound 3 and TCF are subjected to a dissolution reaction, and TEC-OH is obtained; and finally, dropwise adding a dichloromethane solution containing 2, 4-dinitrofluorobenzene into a dichloromethane solution containing TEC-OH and triethylamine, and reacting to obtain the probe TEC-H2S. The colorimetric-fluorescent near-infrared probe TEC-H2S is successfully designed and synthesized on the basis of an intramolecular charge transfer (ICT) mechanism and is used for specific detection of H2S, and a sensing technology with a great application prospect is provided for H2S detection.

The invention discloses a synthesis method of 1-bromoethyl acetate, which belongs to the technical field of synthesis of medical intermediates, and comprises the following steps: slowly dripping a hydrobromic acid aqueous solution into phosphorus tribromide to obtain a hydrobromic acid aqueous solution containing phosphorous acid; slowly adding a hydrobromic acid aqueous solution containing phosphorous acid into vinyl acetate to obtain a reaction solution; adding cyclohexane for extraction, washing with a saturated sodium hydroxide solution and distilled water until the solution is neutral, separating out a lower-layer organic phase, and drying; concentrating the dried organic phase under reduced pressure, and evaporating to remove the solvent to obtain mother liquor; and continuously carrying out reduced pressure distillation on the mother liquor to obtain the 1-bromoethyl acetate. The synthesis method of the 1-bromoethyl acetate has the advantages that the process conditions are mild, the reaction temperature is 15-25 DEG C, the operation is simple and convenient, the purity of the prepared 1-bromoethyl acetate is more than 99.5%, and the yield is 85.1-90.2%.