1236results about How to "Atom economy is high" patented technology

The invention discloses a preparation method of organopolysiloxane resin. The preparation method includes the steps of (1), taking alkoxyorganosilane, an end-capping reagent and an acidic compound as preparation raw materials; (2), feeding the preparation raw materials with uniform stirring, wherein the feeding molar ratio of the end-capping reagent to the alkoxyorganosilane to the acidic compound is (0-40):1:(0.2-5); (3), adjusting the temperature at 40-150 DEG C at which condensation polymerization reaction is conducted for 2-20 hours; (4), terminating the condensation polymerization reaction, adjusting a reaction mixture to be neutral, and purifying a reaction product so as to obtain the organopolysiloxane resin. The preparation method of the organopolysiloxane resin has the advantages of environmental protection and no pollution during production, low energy consumption, short period, high product yield and the like and is more excellent in performance.

The invention provides a method of applying a low metal loading catalyst for preparing glycol and propylene glycol from carbohydrate, including cellulose, starch, semi-cellulose, cane sugar, glucose, fructose, fructosan, xylose, and soluble xylo oligosaccharide. In the method, carbohydrate is taken as the raw material, the compound catalyst is composed of catalytic active components selected from one or more components from following components: highly-disperse and low-loading ruthenium, inorganic compounds, organic compounds, and complex of tungsten, or simple substance tungsten, then one-step catalytic conversion process is carried out under the hydrothermal conditions: temperature of 60 to 350 DEG C, and hydrogen pressure 0.1 to 15 MPa, and the high-efficient, high-selective and high yield preparation of glycol and propylene glycol from carbohydrate is achieved. The method takes highly-disperse and high stability low loading Ru-based catalyst as the reaction catalyst, so the usage amount of value metals is reduced, the loss of catalyst carrier is slowed down, and the recycle rate of Ru-base catalyst is increased. The catalyst has the prominent advantages of high activity, high selectivity, and very high cyclicity. Compared to other technologies, which prepare polyol from carbohydrate, the method has the advantages of simple reaction process, high efficiency, good stability of catalyst, and multi-circulation, and has very vast industrial application value.

The invention belongs to the technical field of biomass conversion utilization, and concretely relates to a method for preparing cyclopentanone by taking biomass resource as a raw material. The method comprises taking furfural coming from biomass as the raw material, taking a hydrogen-containing gas as a reducing agent, and in the presence of a metal supported type catalyst, performing hydrogenation rearrangement reaction in a high-pressure reaction kettle or a fixed bed reactor, so as to obtain cyclopentanone in one step, wherein the carrier of the metal supported type catalyst is selected from Nb2O5, H-ZSM-5 molecular sieve, HY molecular sieve, Fe2O3, ZrO2, Al2O3, SiO2, CeO2, MgO, active carbon, and TiO2 in various crystal forms, the active composition is selected from Au, Pt, Ru, Rh, Pd, Ir, Ni and Cu, and the active composition load capacity is 0.1-5% of the catalyst. The method is mild in reaction technological conditions, and cheap and easily-available in raw materials, is capable of realizing quantitative conversion of furfural to cyclopentanone, and belongs to an environment-friendly green chemical technology.

The invention provides a preparation method of a CF2O-contained monomer liquid crystal compound. The preparation method comprises the following steps of (1) with a compound with a structure as shown in the formula I as a raw material, reacting under the catalytic action of a zinc reagent and copper salt and in the existence of a solvent to generate a compound with a structure as shown in the formula II; (2) enabling the compound with the structure as shown in the formula II and a fluorinated reagent to be subjected to fluoridation in the existence of the solvent to generate a compound with a structure as shown in the formula III; (3) enabling the compound with the structure as shown in the formula III and boric acid as shown in the formula IV to be subjected to SUZUKI coupled reaction in the existence of the solvent to obtain the CF2O-contained monomer liquid crystal compound with a structure as shown in the formula V, wherein the CF2O-contained monomer liquid crystal compound with a structure as shown in the formula V is as shown in the specification.

The invention discloses a 3-cyclohexyl-1,1-dimethylurea compound as well as a preparation method and application thereof. The 3-cyclohexyl-1,1-dimethylurea compound is used for preparing an antischizophrenic drug cariprazine. Compared with the prior art and report literatures, the preparation method of the 3-cyclohexyl-1,1-dimethylurea compound has the remarkable advantages of being free of removal of protecting groups such as Boc group, high in atom economy, low in cost and easy in getting of raw materials, mild in reaction condition, stable in yield, simple and convenient to operate, controllable in product quality, high in product purity, less in three waste pollution and easy to produce industrially. The structure formula of the 3-cyclohexyl-1,1-dimethylurea compound is as shown in (I) in the specification.

The present invention provides a new synthesis method of a baricitinib compound 11. According to the present invention, by using a compound 1 as a staring raw material, the amino group is protected by directly using ethanesulfonyl chloride, and direct cyclization is directly performed by using the effect of an alkali to obtain a key intermediate compound 3 so as to avoid the use of other protection groups and substantially improve the route efficiency and the atomic economy; during the compound 5 preparation, a Wittig reaction is performed by using triphenylphosphine acetonitrile so as to avoid the use of strong alkali and improve the reaction yield; the completely-new neopentyl glycol borate derivative compound 8 has good stability and good crystallinity so as to simplify the separation and purification process; and the route is simple to operate and has the high yield, the purity of the obtained product is high, and the synthesis method is suitable for amplification production. The formulas 1-11 are defined in the specification.

The invention discloses a chirality dihydrogen silane compound. The chirality dihydrogen silane compound is as shown in the formula IV. In the formula IV, X represents a chiral carbon atom. The invention further discloses a synthetic method for the chirality dihydrogen silane compound. The method comprises the following steps: using olefin shown in the formula I and silane shown in the formula II as raw materials, and using a chiral CoX2-OIP complex compound as a catalyst, in the existence of a reducing agent, reacting to obtain the chirality dihydrogen silane compound shown in the formula IV. The synthetic method is suitable for different types of the olefins, the reaction condition is moderate, the operation is simple and convenient, and the atomic economy is high. The reaction does not need to be added with any other toxic transition metal ions, the reaction yield is better and is 53%-97% generally, and the enantio-selectivity is higher and is 81%-99% and gt generally. The provided chirality dihydrogen silane compound shown in the formula IV can be used for synthesizing a chiral alcohol compound, a chiral silicon alcohol compound, a chiral polysubstituted silane compound and so on.

The invention discloses nitrilase from brassica rapa, encoding genes and an application of the encoding genes to the preparation of pregabalin chiral intermediate (S)-3-cyan-5-methylhexanoic acid through biocatalysis, and an amino acid sequence of the nitrilase is shown as SEQ ID NO:1. The invention provides novel nitrilase for preparing the (S)-3-cyan-5-methylhexanoic acid with high region and high stereoselectivity through hydrolysis, the concentration of hydrolysis substrates of the nitrilase can reach more than 1 M, and an ee (enantiomeric excess) value is kept more than 99 percent. The pregabalin important chiral intermediate (S)-3-cyan-5-methylhexanoic acid can be prepared through the nitrilase; a preparation method of the (S)-3-cyan-5-methylhexanoic acid has the advantages of high atom economy, mild conditions, environmental friendliness and the like and has high industrial application potential.

The invention relates to a method for preparing epoxy butane, which comprises the following step: in an isopropyl benzene solution containing 25 wt% of cumene hydroperoxide solute, preparing epoxy butane from butylene oxide by using the cumene hydroperoxide solute as an oxidizer and a titanium-silicon molecular sieve with three-dimensional pore canal structure as a catalyst, wherein the fixed bed reaction conditions are as follows: the mole ratio of butylene to the cumene hydroperoxide solute is (5.0-12.0):1, the weight hourly space velocity of the cumene hydroperoxide is 1.0-5.0 h<-1>, the reaction pressure is 1.0-6.0 MPa, and the temperature is 60.0-120.0 DEG C. The catalyst is the titanium-silicon molecular sieve with three-dimensional pore canal structure; the molecular sieve has hysteresis loop on the low-temperature nitrogen adsorption and desorption isotherm; the average pore size is 2.0-8.0nm, and the specific area is 650.0-1100.0 m<2>/g; and the catalyst has the advantages of favorable activity and high epoxy butane selectivity, and can be widely popularized and applied to industrial production of epoxy butane by butylene epoxidation.

The invention discloses a method for preparing a nitro compound from a low-valent nitric oxide. The method comprises that a low-valent nitric oxide such as nitric oxide, nitrogen dioxide, nitrous oxide, nitrogen trioxide, dinitrogen tetroxide and the like react with an alicyclic compound, an aromatic compound or a heterocyclic compound through promoting effects of molecular oxygen and effects of catalysts comprising a transition metal oxide, a triphenylphosphine metal organic complex, transition metal ion clay and heteropoly acid salts such as aluminosilicate, silicoaluminophosphate, sodium phosphomolybdate and the like. The method can replace the traditional industrial method for preparing a nitro compound from a high-valent (V-valent) nitrogen compound such as nitrogen pentoxide, hydrogen nitrate, nitric acid salts, nitric acid esters and the like. The method improves an atom utilization rate of a reaction in industrial nitration preparation of a nitro compound, and has atom economic characteristics of industrial preparation of a nitro compound.

The invention belongs to the field of organic synthesis, and particularly discloses a preparation method of a 3-o-alkylation quinoxaline-2(1H)-ketone compound. The method includes the steps that a quinoxaline-2(1H)-ketone compound, an ether compound, alkaline, an oxidizing agent and a photocatalyst are added into a reacting bottle and react for 18-30 hours under illumination of a visible light lamp, after the reaction is ended, extracting treatment and concentrating treatment are performed, and the 3-o-alkylation substitution quinoxaline-2(1H)-ketone compound is obtained after column chromatography isolation purification treatment is performed. According to the method, the raw materials are easy to obtain, reaction conditions are simple and convenient to implement, using of metal reagents,high temperature and complex operation are avoided, reaction time is short, energy consumption is low, the compatibility of substrate functional groups is good, the safety and efficiency of the reaction are high, and high application values are obtained.

The invention belongs to the field of organic and medicine synthetic chemistry, and discloses a tridentate nitrogen phosphine ligand. The tridentate nitrogen phosphine ligand has a structure shown ina formula I which is shown in the attached figure, wherein R1 is toluene sulfonyl or 2,4,6-triisopropylbenzenesulfonyl, and R2 is aryl or substituted aryl. The invention also discloses a complex of the tridentate nitrogen phosphine ligand; the complex is prepared by mixing the tridentate nitrogen phosphine ligand and a transition metal complex; the complex is used for asymmetric catalytic hydrogenation of ketone. The tridentate nitrogen phosphine ligand has the advantages that 1, the synthesizing is easy, and the chiral ligand can be prepared by only two to three reaction steps; 2, the ligandis stable, the series of ligand is not sensitive to water and oxygen, and the convenience in storage and use is realized; 3, the catalyzing effect is good, and the catalyst can be used for realizing 100% of conversion and 99% of stereo selectivity on most of suitable primers; 4, the atom economy is high, and the activity of the catalysis system is higher; for most of suitable primers, the conversion number reaches more than 10000, and the maximum conversion number reaches 200000.

The invention discloses an organic electrosynthesis method of a phenothiazine/phenoxazine compound. The organic electrosynthesis method adopts an organic electrosynthesis means for a compound shown ina formula I and a compound shown in a formula II to prepare the phenothiazine/phenoxazine compound. The organic electrosynthesis method disclosed by the invention has the beneficial effects that a target product shown in a formula III can be obtained by directly activating C-H without need of expensive halogenated raw materials and additional reduction and substitution processes, so that the process flow is obviously shortened, the operation is simplified, the preparation efficiency is improved, and the production cost is reduced; the reaction condition is simple, mild and environmentally friendly, the atom economy is high, the adaptation range of a reaction substrate is wide, and the yield of a target product is high.

The invention provides a method for synthesizing a 1,2,4-triazolohetercyclic compound. The method comprises the following steps: dissolving a 2-hydrazinohetercyclic compound (I) and an aldehyde compound (II) into acetonitrile A; stirring at 25 DEG C to 80 DEG C and reacting for 1h to 8h; then adding tetrabutylammonium tetrafluoroborate, acetonitrile B and water; taking a graphite carbon rod as an anode and a platinum sheet as a cathode; switching on a power supply and electrifying for 3h to 8h, wherein the current strength is 15mA/mmol to 30mA/mmol according to the amount of substance of the aldehyde compound (II); carrying out post-treatment on a reaction solution to obtain the product 1,2,4-triazolohetercyclic ring compound (III). The method has the advantages of simple reaction system, easiness for obtaining raw materials and high total yield; the 2-hydrazinohetercyclic compound and the aldehyde compound are subjected to electrochemical catalysis to obtain the 1,2,4-triazolohetercyclic compound in one step; only one water molecule and one hydrogen molecule are removed and the atomic economy is extremely high; the formula is shown in the description.

The present invention belongs to the technical field of organic synthesis, and particularly relates to a method for carrying out a reaction on a methylenecyclopropane derivative and an ether compound C(sp<3>)-H bond. According to the present invention, a methylenecyclopropane derivative represented by a formula II and an ether compound represented by a formula III are subjected to a reaction in the presence of a free radical initiator to obtain a 1,2-dihydronaphthalene derivative represented by a formula I, wherein the free radical initiator is the mixture comprising one or a plurality of materials selected from TBHP (tert-butyl hydroperoxide), CHP (Cumyl hydroperoxide), and THAP (tert-amyl hydroperoxide). The formulas I, II and III are defined in the specification.

The invention discloses a method for preparing a dihydropyrrole derivative and an intermediate pyrrolidine thereof, and relates to the preparation of the pyrrolidine and the dihydropyrrole derivative. Firstly, a diazocompound, amine, beta, gamma-unsaturated-alpha-keto ester with the mol ratio of 1.2 to 1.2 to 1 to 0.01 are weighed as raw materials, metal Lewis acid is taken as a catalyst, the diazocompound is decomposed to form metal carbine through a three-component tandem reaction under the catalysis of the metal Lewis acid, ammonium ylide obtained by in-situ formation of the metal carbine and the amine is captured by the beta, gamma-unsaturated-alpha-keto ester through the 1, 4-addition mode, then a corresponding intermediate pyrrolidine derivative is obtained through intra-molecular condensation, finally the pyrrolidine derivative is mixed with an organic solvent, then an organic acid catalyst is added to form a reaction system, and then the corresponding dihydropyrrole derivative is obtained through the water entrainment of a water segregator. The method has the advantages of high atom economy, high efficiency, high yield and so on, and has safe and simple operation. The prepared pyrrolidine and the dihydropyrrole derivative are widely applied to the field of pharmaceutical and chemical industries.

The invention belongs to the technical field of a macromolecular polymer, and discloses a multi-component polymerization method based on alkyne and sulfonyl azide as well as a sulfonyl-containing polymer and application. The multi-component polymerization method comprises the step of performing multi-component polymerization reaction on a binary alkynyl compound, a binary sulfonyl azide compound and a third component compound under the protective atmosphere and through the effect of a univalent copper catalyst to obtain the sulfonyl-containing polymer, wherein the third component compound is acyanophenyl compound containing hydroxyl or amino, a formyl-containing thiophenol potassium compound, an amino-containing benzoyl compound, ammonium salt, ammonia, thiocyanate or selenium cyanate. The method is mild in polymerization conditions, simple in process, high in polymerization efficiency, large in product molecular weight and high in atom economy; furthermore, a functional element containing the complex structure can be constructed in situ simply and efficiently. The obtained sulfonyl-containing polymer is applied in the fields of fluorescence detection, metal ion detection, organicphotoelectric materials and antibacterial materials.

The invention discloses a method for preparing fatty acyl potassium glycine and a composition containing the surfactant, and belongs to the technical field of fine chemical engineering. According to the technique for synthesizing a fatty acyl potassium glycine type surfactant, fatty acid methyl ester of a natural fat resource is taken as a raw material for synthesizing the fatty acyl potassium glycine type surfactant, that is, fatty acid methyl ester and potassium glycine react in the presence of a phase shifting catalyst PEG2000 to prepare fatty acyl potassium glycine and the composition containing the surfactant. The method is high in raw material utilization rate, high in yield, high in active matter content, high in surface activity, simple in synthesis route, and free of environment pollution and is a green synthesis technique, and products can be directly used without being separated or purified. The invention further discloses a surfactant composition containing the fatty acyl potassium glycine.

The invention provides a novel method for preparing chiral alpha-hydroxy amide through asymmetric hydrogenation of pro-chiral alpha-keto-amide using a novel tridentate nitrogen phosphine ligand to prepare a series of chiral alpha-hydroxy amide compounds. The method comprises the following steps of performing asymmetric hydrogenation reaction by adding prochiral alpha-keto-amide and a base under a hydrogen gas atmosphere in the presence of a catalyst to obtain chiral alpha-hydroxy amide, wherein the catalyst is prepared by complexing a metal iridium salt and the chiral ligand. The ligand used in the method is easy to synthesize, and the reaction has the characteristics of high enantioselectivity, high yield and high conversion number. Most of the substrates have a conversion rate of 99% or more under the condition of ten thousandth catalyst dosage and have the ee value of 97% to 99% or more, the highest conversion number reaches to 100,000, and extremely high industrialization value is obtained.