705 results about "One pot reaction" patented technology

The present invention provides herein a two-step process for preparing pharmaceutically pure quetiapine and salts thereof by obtaining the starting material 11-chloro-dibenzo-thiazepine followed by reacting the 11-chloro-dibenzo-thiazepine with 1-(2-hydroxyethoxy)ethylpiperazine, or its salt, in the presence of an inorganic or organic base in an organic solvent or in a two-phase solvent system. The present invention provides also a novel, one-pot reaction process for preparing pharmaceutically pure quetiapine and salts thereof. The two processes provided herein can be easily, conveniently and inexpensively scaled-up.

Applicant has discovered an in situ method of preparing quaternary ammonium methocarbonate salts and quaternary ammonium alkylcarbonate salts in high yield from tertiary amines, methanol, and at least one of a cyclic carbonate, an aliphatic polyester (such as a polycarbonate), or an ester (such as a carbonate ester), and their subsequent conversion to quaternary ammonium bicarbonates, quaternary ammonium carbonates or both in a one-pot reaction. According to one embodiment of the invention, the method includes reacting an amine and methanol with at least one of a cyclic carbonate and an aliphatic polyester to yield a quaternary ammonium methocarbonate. This method does not produce or require the handling of corrosive quaternary ammonium hydroxides. Another embodiment is a method of preparing quaternary ammonium alkylcarbonate salts by reacting tertiary amines, methanol, and an ester. The quaternary ammonium methocarbonate or alkylcarbonate can be converted to the corresponding bicarbonate, carbonate, or mixture thereof by methods known in the art.

Process for preparing polymer-reinforced silica aerogels which comprises a one-pot reaction of at least one alkoxy silane in the presence of effective amounts of a polymer precursor to obtain a silica reaction product, the reaction product is gelled and subsequently subjected to conditions that promotes polymerization of the precursor and then supercritically dried to obtain the polymer-reinforced monolithic silica aerogels.

The present invention relates to a method for preparing a CdX (X= Se or Te) quantum dot nano material with high quantum yield in an aqueous phase by using simple operation conditions, and belongs to the field of nano material preparation. The preparation method does not require nitrogen as a protective gas, or a buffer solution, or a particular ligand, or a large amount of hydrazine hydrate as a reducing agent, or a special post-treatment. In the aqueous phase, a thiol compound is used as a ligand; cadmium salt and potassium tellurite (selenite) are selected respectively as a cadmium source and a tellurium (selenium) source; and sodium borohydride is used as a reducing agent. The water-soluble CdTe (CdSe) quantum dot with quantum yield up to 83% can be prepared from a one-pot reaction.

The present invention relates to a process of reducing sulfur- or nitrogen-containing compounds and also producing oxygenates, which can be used as an excellent octane booster in the reformulated gasoline and as a cetane booster for the future oxygenated diesel in a one-pot reaction.

The invention discloses an enzyme-chemocatalysis racemization removing preparation method for L-glufosinate-ammonium. According to the method, a one-pot reaction manner is adopted, under the molecular oxygen, immobilization D-amino acid oxidase catalyzes D-enantiomer in an enantioselectivity mode into 2-imino-4-(hydroxy methyl phosphonyl) butyric acid in a dehydrogenation mode, and palladium-ammonium formate catalyzes 2-imino -4-(hydroxy methyl phosphonyl) butyric acid into DL-glufosinate-ammonium in an in-situ reduction mode. Hydrogen peroxide produced in the process is efficiently decomposed into water and oxygen through catalase. Complete reacemization removing of DL-glufosinate-ammonium and efficient preparing of L-glufosinate-ammonium are achieved through biological oxidation-chemical reduction circulation. The method has the advantages that the process is simple, cost is low, environmental friendliness is achieved, and energy is saved. High-concentration DL-glufosinate-ammonium can be converted into L-glufosinate-ammonium. The yield is 90%, the optical purity of the product is 99%, and the method is suitable for industrial production of L-glufosinate-ammonium.

The invention discloses a method for preparing a cellulose ester grafted aliphatic polyester copolymer. The method comprises the following steps: 1) preparing a cellulose / ionic liquid solution by using cellulose as a raw material; 2) conducting a homogeneous acylation reaction of cellulose in the cellulose / ionic liquid solution to obtain partially substituted cellulose ester; and 3) further grafting aliphatic polyester to the partially substituted cellulose ester to obtain cellulose ester grafted aliphatic polyester copolymer. Compared with the existing method, the method has obvious advantages that cellulose with wide source is directly used as raw material to prepare the cellulose ester grafted aliphatic polyester copolymer by a one-pot reaction, without separation and purification of intermediate cellulose ester, and that the entire production process is greatly simplified, and has simple production process and easy operation. The cellulose ester grafted aliphatic polyester copolymer product produced by the method provided by the invention can be used for spinning, film making and molding parts, and also can be used as a compatibilizer for coating, paint, polymer and composite material.

The invention relates to a method for preparing fluorescence color adjustable carbon dots. According to the method, a diphenol compound is used as a carbon source, and under the action of an oxidizingagent, a carbon dot mixed liquor is generated by a solvothermal one-pot reaction; and then, the carbon dot mixed liquor is purified by column chromatography to obtain the carbon dots emitting variousfluorescence colors. By regulating the combination of the diphenol compound and the oxidizing agent, the fluorescence colors of the carbon dots are adjusted. By the method, long-wavelength luminescence of the carbon dots can be realized, and quantum efficiency is improved. Quantum efficiency of the carbon dots having blue fluorescence color is 66%, quantum efficiency of the carbon dots having green fluorescence color is 81%, quantum efficiency of the carbon dots having yellow fluorescence color is 36%, and quantum efficiency of the carbon dots having red fluorescence color is 7%.

The invention discloses a preparation method of 1T-phase molybdenum disulfide. The preparation method comprises the step of performing a hydrothermal reaction on an aqueous solution comprising a molybdenum source, a sulfur source and an ammonia source at 160-220 DEG C to prepare the 1T-phase molybdenum disulfide. The ammonia source is organic quaternary ammonium salt and / or inorganic ammonia salt. According to the preparation method disclosed by the invention, under the synergistic effect of the ammonia source and the hydrothermal reaction temperature, the 1T-phase molybdenum disulfide can be prepared through a one-pot reaction. The preparation method is simple, high in production efficiency and safe in preparation process.

This invention provides one-pot reaction for digesting polycarbonate waste with alkylene glycol in the presence of a basic catalyst at 180° C. under normal atmospheric pressure. The digested product mixture was found to consist of bisphenol A (BPA) and monoalkoxylated and bisalkoxylated diols of BPA. Alkoxylation of BPA and monoalkoxylated diols of BPA is performed by adding urea or urea derivative (or carbonic acid ester or amine ester) to the digested product mixture at a high temperature under normal atmospheric pressure to obtain the final product, i.e., bisalkoxylated diols of BPA in high yield. The bisalkoxylated diols of BPA may be used as raw materials to synthesize polymer such as polyurethane (PU) or polyester.

The invention belongs to the technical field of preparation of catalysts and particularly relates to a reduced graphene supported molybdenum or tungsten carbide catalyst and a preparation method and application thereof. The preparation method of the reduced graphene supported molybdenum or tungsten carbide catalyst comprises the following steps: (1), synthesizing a heteropolyacid-polymer conductor / reduced graphene composite through a one-pot reaction method by using molybdenum- or tungsten-containing heteropolyacid, a polymer conductor and graphene as raw materials; (2), under the protection of an inert gas, thermally treating at 700-1100 DEG C for 2-5 h, and cooling and pickling to obtain the reduced graphene supported molybdenum or tungsten carbide catalyst. The preparation method of the catalyst is simple, the presence of a unique structure provides a great limitation on the agglomeration of molybdenum or tungsten carbide nanoparticles and an enhancement in their dispersity, excellent hydrogen production from water electrolysis is shown, and the preparation method is also applicable to the fields of studies such as energy storage and conversion studies for electrocatalytic reduction of oxygen, lithium ion batteries and the like.

A process is provided for the semi-synthesis of taxane intermediates useful in the preparation of paclitaxel and docetaxel, in particular, the semi-synthesis of protected taxane intermediate in a one pot reaction of protecting the C-7, 10 and attaching a side chain at C-13 position and subsequently deprotecting the group to form paclitaxel or docetaxel, and intermediates used therein.

The invention discloses a method for synthesizing a flame retardant hexaphenoxy cyclotriphosphazene. The method is characterized by comprising the following steps of: performing a one-pot reaction on hexachlorocyclotriphosphazene, phenol, alkali metal hydroxides and other raw materials in a solvent system consisting of aromatic hydrocarbon or aryl halide and water by adopting noncyclic polyether as a catalyst at the temperature of between 20 and 30 DEG C for 3 to 5 hours; heating to the temperature of between 80 and 100 DEG C, reacting for 3 to 5 hours; reclaiming hydrated aromatic hydrocarbon or aryl halide through cooling, separation, washing and depressed pressure distillation after the reaction is completed; and cooling and coagulating the residues to obtain a white crystal solid powder product, wherein the yield is over 95 percent. The method has the characteristics of short reaction time, low cost, good quality and the like, is simple and safe in operation, and is environmentally-friendly and suitable for industrial production and application.

The invention relates to a preparation method for ionic liquid, especially to a one-step method for synthesis of a quaternary ammonium or quaternary phosphonium compound. According to the method, a nitrogen compound or phosphorus-containing compound, a proton compound and carbonic ester are added into a reactor together for a one-step reaction so as to synthesize corresponding quaternary ammonium or quaternary phosphonium ionic liquid, wherein the reaction is a one-pot reaction involving three reactants. The invention also provides a lithium ion secondary battery of the ionic liquid prepared by using the preparation method. The preparation method for the ionic liquid can broaden the selection scope of preparation raw materials for the ionic liquid, so the varieties of synthesized ionic liquid are enriched; and the preparation method utilizes nontoxic and harmless raw materials, has mild reaction conditions, low requirements on production equipment and low production cost, and meets demands of green industry and large-scale industrial production.

The invention relates to a simple and quick method for synthesizing an improved vitamin B1 intermediate 2-methyl-4-amino-5-aminomethylpyrimidine. The method comprises the following steps: condensing 3-alkyl (aryl) formamido-propionitrile serving as a raw material with acetamidine in the catalytic action of lewis acid; cyclizing with trimethyl orthoformate, and hydrolyzing under an alkaline condition to prepare the vitamin B1 key intermediate 2-methyl-4-amino-5-aminomethylpyrimidine. The four reacting processes are performed in sequence by a one-pot reaction, and the product in each step does not need to be separated and purified. According to the method, highly carcinogenic o-chloroaniline or other small molecular aniline compounds are not used, residues of o-chloroaniline compounds in the vitamin B1 product can be eliminated. Furthermore, the preparation process is short and convenient in flow, small in wastewater amount and high in yield.

This invention provides one-pot reaction for digesting polycarbonate waste with alkylene glycol in the presence of a basic catalyst at 180° C. under normal atmospheric pressure. The digested product mixture was found to consist of bisphenol A (BPA) and monoalkoxylated and bisalkoxylated diols of BPA. Alkoxylation of BPA and monoalkoxylated diols of BPA is performed by adding urea or urea derivative (or carbonic acid ester or amine ester) to the digested product mixture at a high temperature under normal atmospheric pressure to obtain the final product, i.e., bisalkoxylated diols of BPA in high yield. The bisalkoxylated diols of BPA may be used as raw materials to synthesize polymer such as polyurethane (PU) or polyester.

The invention discloses a method for synthesizing an important intermediate 4-amino-3-(4-phenoxy-phenyl)-1H-pyrazolo[3,4-d]pyrimidine of Ibrutinib. The method comprises the following steps: step one, condensing malononitrile and triethyl orthoformate and then carrying out a one-pot reaction with hydrazine hydrate to obtain 5-amino-4-cyano-pyrazole; step two, condensing the 5-amino-4-cyano-pyrazole with formamide to prepare a compound of formula (II) 4-amino-1H-pyrazolo[3,4-d]pyrimidine; step three, carrying out a bromination reaction of the compound of formula (II) and brominating agent to obtain a compound of formula (III) 4-amino-3-bromine-1H-pyrazolo[3,4-d]pyrimidine; step four, carrying out a Stille reaction on the compound of formula (III) and trimethyl p-phenoxy phenyltin under the catalyst effect of metal palladium to prepare a compound of formula (I) 4-amino-3-(4-phenoxy-phenyl)-1H-pyrazolo[3,4-d]pyrimidine. According to the method for synthesizing the important intermediate 4-amino-3-(4-phenoxy-phenyl)-1H-pyrazolo[3,4-d]pyrimidine of Ibrutinib provided by the invention, raw materials are low in price and easily obtained, the reaction conditions are moderate, the operation is simple and convenient, the method is suitable for industrial production, and a new way is provided for preparing Ibrutinib and intermediate.

The invention discloses carbon microsphere solid acid formed by one-step fructose hydrothermal synthesis and applied to a catalyzed hydrolysis process of cellulose, and belongs to the field of conversion and utilization of biomass resources and energy. A carbon microsphere solid acid catalyst disclosed by the invention has the molecular formula of CH0.0847O0.523S0.00840. The preparation conditions of the catalyst are mild; through one-pot reaction of fructose and sulfo salicylic acid under the hydrothermal condition of 150 DEG C, the preparation of solid microspheres and the loading of sulfo groups are realized simultaneously; the defects that a large amount of concentrated sulfuric acid is used and a large amount of sulfuric acid waste liquid is produced in a conventional process of preparing the solid acid by soaking the concentrated sulfuric acid by using activated carbon are overcome. The prepared carbon microsphere solid acid has high the catalytic activity on the hydrolysis of the cellulose. The solid acid catalyst has mild preparation conditions, no pollution, no corrosion and high activity, and can be used repeatedly for the hydrolysis of the cellulose. The carbon microsphere solid acid is prepared from the fructose and is applied to efficient hydrolysis of the cellulose; a new way is provided for the high value of the biomass resources.

The invention discloses a method for preparing hexitol or hydroxy-acetone, which comprises the steps as follows: cellulose reacts with glucose or fructose in water under the action of hydrogen atmosphere and catalytic agents, so as to obtain hexitol or hydroxy-acetone; the catalytic agents are supported metal catalysts; active constituents of the supported metal catalysts are metal modified by modifiers; the metal is any one of Pt, Ru, Ni and Cu; and a carrier of the supported metal catalysts is any one of Al2O3, TiO2, ZrO2, SiO2 and activated charcoal. The provided method selectively obtains hexitol or hydroxy-acetone through a one-pot reaction based on cellulose and glucose or fructose, achieves simple process, rapid reaction, high efficiency and energy conservation, and is easy to industrialize; the catalytic agents can be recovered and recycled, so that the cost is saved, and environmental protection can be achieved; in addition, the method has low requirements on equipment, cannot corrode equipment, and achieves low investment.

The invention relates to a preparation method and an application of a hydrophobic starch sulfate ester in a cement water-reducing agent, and belongs to the fields of chemistry and chemical engineering. The preparation method comprises the following steps: adding a sulfamic acid, starch, urea, aliphatic tertiary alcohol or aryl methyl alcohol and water into a reactor under the conditions that the molar ratio of the sulfamic acid to the starch is (0.5-3.0):1, the molar ratio of the urea to the starch is (0.1-3.0):1, the molar ratio of the aliphatic tertiary alcohol or the aryl methyl alcohol to the starch is (0.1-1) and the adding amount of the water accounts for 10% to 30% of the dry weight of the starch; and reacting for 1 to 10 hours at a temperature of 80 DEG C to 150 DEG C, thereby obtaining the hydrophobic starch sulfate ester in which the sulfonyl substitution degree is between 0.04 and 0.89 as well as the alkyl substitution degree is between 0.01 and 0.2. The hydrophobic starch sulfate ester is applied to the cement water-reducing agent, wherein the mass percent of the hydrophobic starch sulfate ester accounts for 0.1% to 1.0% of that of cement. According to the method, a dry method and one-pot reaction are adopted, so that the environmental pollution caused by the application of an organic solvent is avoided. Thus, the production cost is decreased.

The invention relates to the field of covalent organic framework materials, and particularly provides a covalent organic framework material and a preparation method and application thereof. Accordingto the method, firstly, a COF material containing an imidazole structural unit is simply synthesized by adopting a three-component one-pot Povarov reaction, and then a structure of strong protonic acid polyion liquid is introduced into a porous framework by cooperating with a one-step post-synthesis modification strategy, so that the COF catalyst with high stability, high-density sulfonic acid group content and quinoline ring points is obtained and is used for efficiently catalyzing a Biginelli reaction. The invention provides a new way for the construction of the high-stability crystalline porous catalytic material.

A method for template-directed sequencing-by-synthesis of an array of target polynucleotide can include:(a) providing an array of target polynucleotides in a fluidic vessel;(b) contacting the array of polynucleotides with a solution comprising (i) polymerization complex and (ii) reversibly terminating and differently labeled A,C,G, and T / U nucleotides;(c) incorporating one of the differently labeled nucleotides, using the polymerization complex, into a chain complementary to at least one of the array of polynucleotides;(d) binding imaging tags to the differently labeled nucleotides of step (c);(e) imaging and storing the identity and position of the imaging tags of step (d);(f) reversing termination (b)-(e);(g) repeating steps (b)-(e) and assembling a sequence for each of the array of target polynucleotides from the stored identity and position of the imaging tags, optionally as a homogeneous or one pot reaction. Additional methods of sequencing target polynucleotides are described herein.

The invention relates to new compounds of the formula, wherein R and R1 are each independently hydrogen, a linear or branched C1-40 alkyl, C2-40 alkenyl or C2-40 alkynyl group, an aryl or C1-40 alkylaryl group or an optionally complex metal ion Mn+ / n wherein n is an integer from 1 to 8; the free valences of the silicate oxygen atoms are saturated by one or more of: silicon atoms of other groups of the formula, hydrogen, a linear or branched C1-12 alkyl group or by cross-linking bridge members R3qM1(OR2)mOk / 2 or Al(OR2)3-pOp / 2 or R3Al(OR2)2-rOr / 2; where M1 is Si or Ti; R2 is linear or branched C1-12 alkyl group; and R3 is a linear or branched C1-6 alkyl group; k is an integer from 1 to 4 and q and m are integers from 0 to 2; such that m+k+q=4; and p is an integer from 1 to 3; and r is an integer from 1 to 2; or other known oxo metal bridging systems; x, y and z are integers such that the radio of x:y+z, varies from 0.00001 to 100,000 with the fragments [O3 / 2SiCH(CH2PO(OR)(OR1))CH2CH2SiO3 / 2]X and [O3 / 2SiCH2CH2PO(OR)(OR1)]Y always present whilst the integer z varies from 0 to 200y. The compounds are useful as catalysts for a wide variety of reactions and have the advantages that they can be prepared in a one-pot reaction and have functional group losding can be tailored to be at a required level. In addition, the compounds have high chemical and thermal stability, fixed and rigid structures, are insoluble in organic solvents, high resistance to ageing, and can easily be purified and reused.

The invention belongs to the field of preparation of chemical raw medicaments, and more in particular relates to an improved preparation method for a phosphodiesterase 5 inhibitor tadalafil. A specific synthesis route is shown in the specification. The method comprises the following steps of performing Pictet-Spengler cyclization reaction and chloroacetyl chloride acylation on starting reactants (D-tryptophan methyl ester hydrochloride and piperonal) to obtain an intermediate product, directly performing subsequent reaction on the intermediate product without purification, preparing an intermediate 1-(1,3-benzodioxol-5-yl)-2-(chloracetyl)-2,3,4,9-tetrahydro-1H-pyridino-[3,4,-B]indol-3-thiophenate methyl by using a one-pot reaction method, performing column chromatography purification to obtain a single cis-isomer, and finally reacting the single cis-isomer with methylamine hydrochloride in the presence of an inorganic base to obtain the tadalafil.

The invention belongs to the field of lithium ion battery materials, and discloses a carbonyl conjugated heterocyclic compound and preparation and application. The carbonyl conjugated heterocyclic compound is N,N'-diphenyl-1,4,5,8-naphthalimide, and has a structural formula shown as a formula (I). A preparation method comprises the following steps: dissolving 1,4,5,8-naphthalenetetracarboxylic dianhydride in a solvent, stirring to mix uniformly, dropwise adding phenylamine and trithylamine, stirring and performing a refluxing reaction until brown precipitate is generated; separating and washing the precipitate, recrystallizing, washing and drying in vacuum to obtain a product. In the preparation method, a product is prepared through a one-pot reaction, and a synthetic method is simple and feasible, is low in cost, has high yield, saves energy and is environment-friendly. The prepared N,N'-diphenyl-1,4,5,8-naphthalimide has high discharging capacity, high cycling stability and high rate performance after thermal treatment, and is a promising positive electrode material for a lithium ion battery. The formula (I) is shown in the description.

The invention discloses a method for catalytically preparing a spiral [cyclopropane-1,3'- indole] compound. According to the method, silicon amino rare earth compounds of [(Me3Si)2N]3Ln(mu-Cl)Li(THF)3 is used as a catalyst for catalytically replacing isatin, phosphite ester and olefin to prepare a product through one-pot reaction; in the catalyst, (Me3Si)2N represents trimethyl silicon amino; Ln represents positive trivalent rare earth metal irons and are one kind of metal irons selected from lanthanum, samarium, gadolinium, erbium or ytterbium; mu- represents a bridge key; THF represents tetrahydrofuran. In the method, the synthesis method of the catalyst is simple; the reaction raw materials are simple and can be easily obtained; the application range of a substrate is wide; the efficiency of the one-pot reaction method is high; the reaction conditions are mild; the yield of most target products can reach 85 percent or higher.

Ternary and quaternary Chalcopyrite CuInxGa1-xSySe2-y (CIGS, where 0≦x and y≦1) nanoparticles were synthesized from molecular single source precursors (SSPs) by a one-pot reaction in a high boiling solvent using salt(s) (i.e. NaCl as by-product) as heat transfer agent via conventional convective heating method. The nanoparticles sizes were 1.8 nm to 5.2 nm as reaction temperatures were varied from 150° C. to 190° C. with very high-yield. Tunable nanoparticle size is achieved through manipulation of reaction temperature, reaction time, and precursor concentrations. In addition, the method developed in this study was scalable to achieve ultra-large quantities production of tetragonal and quaternary Chalcopyrite CIGS nanoparticles.

A process for the preparation of a 5,5'-bi-1H-tetrazole diammonium salt by dropwisely adding the aqueous hydrogen peroxide to which a small amount of weakly acidic substance has been added, to a starting aqueous solution containing hydrogen cyanide or sodium cyanide or potassium cyanide, sodium azide and a catalytic amount of copper sulfate preferably at a low temperature to maintain the pH of the reaction solution over a range of from 5 to 6, heating the reaction solution to effect the oxidation and cyclization reaction, reacting the reaction product with ammonium chloride or an aqueous solution thereof, and recovering the formed ammonium salt in the form of sparingly soluble crystals. The desired product is obtained in a high yield and in a high purity from the starting materials which are cheaply available and are easy to handle through a decreased number of steps, i.e., through a one-pot reaction without requiring cumbersome after-treatment.