17 results about "Electrophilic addition" patented technology

The invention provides a chiral delta-lactam compound as well as a preparation method and application thereof. The preparation method of the chiral delta-lactam compound comprises the following steps: taking a 1, 4, 2-dioxazole-5-ketone derivative and a nucleophilic reagent as raw materials, and reacting under the action of a chiral metal catalyst and an additive to generate the chiral delta-lactam compound. According to the synthesis strategy, under the catalysis of a chiral Ir (III) catalyst, an olefin part in a substrate molecule and electrophilic metal nitrogen are subjected to an electrophilic addition reaction to generate a carbocation intermediate, then 1, 2-negative hydrogen migration is carried out under the promotion of a chiral ligand, more stable aza carbocations are formed, and the chiral Ir (III) compound is synthesized. And a nucleophilic reagent captures the compound to form a delta-lactam compound containing a continuous gamma, delta-chiral center. The method has excellent yield, diastereomer selectivity and enantiomer selectivity, and is compatible with various carbon, nitrogen and oxygen nucleophilic reagents and biological related molecules. The invention provides a brand-new efficient route for synthesis of the chiral delta-lactam compound.

The invention provides a preparation method of hexafluorobutadiene, which comprises the following steps: 1) carrying out electrophilic addition reaction on chlorotrifluoroethylene and liquid bromine at normal temperature and normal pressure to generate 1, 2-dibromo-1-chloro-1, 2, 2-trifluoroethane; 2) mixing zinc powder, 1, 2-dibromo-1-chloro-1, 2, 2-trifluoroethane and an aprotic polar solvent, and carrying out a reaction so as to obtain a zinc reagent containing 1-chloro-2-bromo-1, 2, 2-trifluoroethyl zinc bromide and 1, 2-dibromo-1, 2, 2-trifluoroethyl zinc chloride; 3) adding a catalyst and a zinc reagent, and carrying out a self-coupling reaction to generate an intermediate product containing 1, 4-dibromo-2, 3-dichloro-1, 1, 2, 3, 4, 4-hexafluorobutane and 1, 2, 3, 4-tetrabromo-1, 1, 2, 3, 4, 4-hexafluorobutane; 4) dehalogenating the intermediate product to generate hexafluorobutadiene; the method has the effects of simple reaction process, relatively low risk, relatively mild reaction conditions and relatively high yield.

The application discloses a preparation method of polyurethane material with high compact crosslinking structure. Biomass seed fiber is extracted by Soxhlet extraction method, electrophilic addition is carried out by introducing an epoxy reagent, O-H in the seed fiber is reserved and hydrophobic regulation is carried out; the seed fiber is mixed with biomass derived polyol by doping method, and high compact crosslinking structure polyurethane material is obtained by polymerization with isocyanate. In the application, the environmentally friendly vegetable oil replaces the petroleum derived polyol, not only the biomass derived polyol mixture containing seed fiber is introduced to generate polyurethane with isocyanate, but also the hydrogen bond is formed between O-H in the seed fiber and the formed polyurethane, the interaction between the matrix and the fiber is ensured, the crosslinking density of the polymer is increased, the overall density is greater than 0.3 g / cm 3 , and the hydrophobicity and thermal insulation of the polymer are improved, the thermal conductivity is less than 0.03 W / (m.K), and the contact angle is greater than 150 degrees.

The invention belongs to the technical field of synthesis of organic compounds, and discloses a synthesis method of a dithiophosphonate compound, which comprises the following steps of: reacting diphenylphosphine, elemental sulfur and an olefin compound or an alkyne compound under the conditions of no catalyst and no solvent to prepare the dithiophosphonate compound, the reaction time is 6-12 hours. According to the invention, diphenylphosphine and elemental sulfur are used as raw materials and can rapidly react to generate dithiophosphonic acid in situ. According to the present invention, the dithiophosphonic acid has strong acidity, such that the dithiophosphonic acid can catalyze the electrophilic addition reaction of the dithiophosphonic acid and the olefin or the alkyne so as to obtain the dithiophosphonate product, the reaction condition of the reaction is mild, the catalyst and the organic solvent are not required, the reaction by-product is less, and the green chemistry requirement is met;

The application discloses a plugging removing agent for stratum pore channels based on diazonium salt and a preparation method and application thereof, and belongs to the technical field of oil field plugging removal. The method comprises the following steps: reducing the surface tension of colloidal plugging material by using a surfactant, dispersing the colloidal plugging material in the pore channel and reducing the adhesion of the plugging material, so as to increase the wettability of the pore channel. The high-temperature condition of the stratum is utilized to make the p-aminobenzoic acid isooctyl ester cation group generated by the decomposition of the diazonium salt, the p-aminobenzoic acid isooctyl ester cation group and electron-rich sites (such as unsaturated carbon-carbon bonds and aromatic rings) in the plugging material are subjected to electrophilic addition or substitution reaction, the molecular structure of the plugging material is loosened, and the adhesion strength of the plugging material is further reduced; the weak acid can gently dissolve the inorganic mineral components in the colloidal plugging material, destroy the internal adhesion structure of the inorganic mineral components, and avoid the pipeline corrosion risk caused by strong acid. The nitrogen gas released by the decomposition of the diazonium salt forms pressure impact in the pore channel, the loosened plugging material is discharged from the pore channel, and the deep plugging removal effect is achieved.

The invention discloses an anemoside B4 derivative as well as a preparation method and application thereof, a compound anemoside B4 (abbreviated as B4 or AB4) is taken as a raw material, and the derivative is prepared by respectively carrying out nucleophilic substitution, electrophilic addition, esterification reaction or amidation and other reactions on C-19 exocyclic double bonds or C-28 carboxyl. The compound is used as an active component to prepare medicines with anti-inflammatory and immunoregulation effects. The invention discloses the effect of the B4 derivative on treating inflammatory diseases such as inflammatory bowel disease, atopic dermatitis, eczema and psoriasis for the first time, and the drug effect of the B4 derivative is superior to that of B4 or clinically common drugs. In addition, the invention also discloses that most B4 derivatives do not show obvious cytotoxicity to macrophages for the first time, can reduce the P-I kappa Ba protein level in LPS and ATP induced macrophage NF-kappa B signaling pathways, inhibit the activation of NLRP3 signaling pathways and obviously reduce the Pro-IL-1beta level (p is less than 0.05), namely inhibit the activation of inflammasome pathways, and the effect is superior to that of B4; the results show that the B4 derivative disclosed by the invention has better anti-inflammatory activity.

The application provides a preparation method of hexafluorobutadiene, 1) under normal temperature and pressure, chlorotrifluoroethylene and liquid bromine are subjected to an electrophilic addition reaction to generate 1,2-dibromo-1-chloro-1,2,2-trifluoroethane; 2) zinc powder and 1,2-dibromo-1-chloro-1,2,2-trifluoroethane are mixed with an aprotic polar solvent to generate a zinc reagent containing 1-chloro-2-bromo-1,2,2-trifluoroethane zinc bromide and 1,2-dibromo-1,2,2-trifluoroethane zinc chloride; 3) a catalyst is added, and the zinc reagent is subjected to a self-coupling reaction to generate an intermediate product containing 1,4-dibromo-2,3-dichloro-1,1,2,3,4,4-hexafluorobutane and 1,2,3,4-tetrabromo-1,1,2,3,4,4-hexafluorobutane; 4) the intermediate product is subjected to dehalogenation to generate hexafluorobutadiene; and the method has the effects of simple reaction process, low danger, relatively mild reaction conditions and high yield.

This invention provides a solid-state hydrogen storage microporous polymer, its preparation method, and its application. The method includes the following steps: Step S1, in an inert gas atmosphere, a cobalt source and ligand are dissolved in an alcohol solvent, and a cobalt metal functional building block is prepared through an electrophilic addition reaction; Step S2, in an inert gas atmosphere, the cobalt metal functional building block obtained in Step S1, an alkyne structural building block, and a catalyst are uniformly dispersed in a reaction solvent, and a covalently bonded porous material is prepared through a cross-coupling reaction; Step S3, the porous material obtained in Step S2 is purified to remove unreacted monomers and catalyst, thus preparing a solid-state hydrogen storage microporous polymer. The solid-state hydrogen storage microporous polymer prepared by this invention not only has significant advantages such as excellent porosity, high pressure resistance, extreme high and low temperature resistance, and ideal hydrogen storage capacity, but also possesses windproof, moisture-proof, intrinsically heat-insulating, and flame-retardant properties. The preparation process is simple and the conditions are mild, making it a high-performance, high-safety solid-state hydrogen storage material.

The synthesis method comprises the following steps: by taking 3, 5-dimethoxyacetophenone as shown in a formula I as a raw material, carrying out Wittig reaction to obtain mixed-configuration trisubstituted olefin as shown in a formula b, carrying out asymmetric hydroboration reaction by taking pinacolborane as a boron source and a chiral CoCl2-TIP complex as a catalyst under the action of a reducing agent, and carrying out recrystallization to obtain the actinomycete ketone key intermediate. The preparation method comprises the following steps: preparing a chiral alkyl boron compound as shown in a formula c, deprotecting an aldehyde acetal group of the chiral alkyl boron compound as shown in the formula c to form an aldehyde group, carrying out intramolecular electrophilic addition reaction to form a ring, carrying out dehydration elimination to prepare a dihydronaphthalene compound as shown in a formula d, and oxidizing to prepare a key intermediate compound of actinomycete ketone as shown in a formula II. The method has the advantages of mild reaction conditions, simple operation, good reaction conversion rate, total yield of 67.2%, and high enantiomer selectivity of 92%. According to the invention, the reaction steps are shortened, the reaction yield is increased by more than 10 times, and good enantioselectivity is still maintained.

This invention provides a multi-stage reaction production process and apparatus for 2-chloroacrylonitrile, relating to the field of 2-chloroacrylonitrile production technology. The process includes: using acrylonitrile as raw material in a chlorination reactor, a crude 2,3-dichloropropionitrile is produced by electrophilic addition reaction with chlorine gas under the action of a chlorination catalyst; the crude 2,3-dichloropropionitrile is fed into a vacuum degassing module to remove dissolved hydrogen chloride and unreacted chlorine gas; the degassed crude 2,3-dichloropropionitrile enters an elimination reactor, where it is further treated with a 10% sodium hydroxide solution to obtain crude 2-chloroacrylonitrile. By using a cleaning tube scraping method, the detection error of the temperature sensor due to the accumulation of impurities over time is reduced, ensuring that the temperature sensor can detect the temperature inside the chlorination reactor in real time and accurately. This solves the problem that the surface of the temperature sensor gradually accumulates impurities over time, leading to increased measurement error.

The utility model discloses a fruit and vegetable disinfection machine, and particularly relates to the field of fruit and vegetable disinfection, the fruit and vegetable disinfection machine comprises a charging bin, the rear end of the charging bin is fixedly provided with a hanger, and the outer surface of the top end of the charging bin is provided with two placing grooves; the first fruit and vegetable disinfection machine and the second fruit and vegetable disinfection machine are placed in the placing groove, and the first fruit and vegetable disinfection machine and the second fruit and vegetable disinfection machine are the same in structure; through electrolysis and water molecule splitting, hydroxyl free radicals (-OH) are temporarily formed in water, organic macromolecular pollutants such as pesticides, antibiotics, hormones, pigments and the like are subjected to dehydrogenation, electrophilic addition and electron transfer reactions under the action of the hydroxyl free radicals until the organic macromolecular pollutants are thoroughly decomposed into water, carbon dioxide and inorganic salt harmless to a human body, then the organic macromolecular pollutants are cleaned with clean water, and the organic macromolecular pollutants are dried. Therefore, the purpose of sterilization and disinfection can be achieved, and the cleaning effect on fruits and vegetables is improved.

The application discloses a preparation process of (1R, 5S)-6,6-dimethyl-3-azabicyclo[3.1.0]hexane, which comprises the following steps: taking 3-methyl-2-butenoic acid ethyl ester as a starting raw material, carrying out an electrophilic addition reaction with bromine in dichloromethane to obtain compound a; taking acetone as a solvent, and performing a removal reaction on the compound a in the presence of anhydrous potassium carbonate to obtain compound b; taking methanol as a solvent, adding sodium methoxide, adding 2-cyanoacetic acid ethyl ester into the system, and performing a nucleophilic addition reaction on the compound b to obtain compound c; taking dimethyl sulfoxide as a solvent, taking lithium chloride as a catalyst, and performing a deesterification reaction on the compound c in the presence of water to obtain compound d; taking methanol as a solvent, taking Raney nickel as a catalyst, adding 7M ammonia / methanol solution, and performing a cyclization reaction on the compound d to obtain compound e; and taking tetrahydrofuran as a solvent, taking lithium aluminum hydride as a catalyst, and reducing the compound e to obtain the product (1R, 5S)-6,6-dimethyl-3-azabicyclo[3.1.0]hexane.

The invention discloses a preparation method of high-purity dihydrooat alkaloid, which comprises two continuous reaction stages of nucleophilic substitution and electrophilic addition and a post-treatment stage of separation and purification, and comprises the following steps: under the condition of nitrogen protection, carrying out nucleophilic substitution reaction on p-hydroxyphenylpropionic acid and carbonyl diimidazole to generate an N-acyl imidazole active intermediate; dropwise adding into an organic solvent of o-aminobenzoic acid without separation to complete electrophilic addition reaction, so as to generate a dihydrooat alkaloid solution with high selectivity; after the reaction is finished, cooling to room temperature, extracting, separating and concentrating an organic phase to separate out a crude product or concentrating a reaction solution until the reaction solution is dry and separating out a crude product in an acidic aqueous solution, and recrystallizing to obtain the high-purity dihydrooat alkaloid. The one-pot process strategy of step-by-step activation and controllable addition is adopted, the reaction has the advantages of being high in chemical selectivity, mild in reaction condition, high in raw material conversion rate and simple and convenient in aftertreatment, phenolic hydroxyl protection is avoided, the problem of high-selectivity amidation is solved, and the preparation cost is effectively reduced.

The invention belongs to the technical field of synthetic fibers, and particularly relates to a preparation method of a procyanidine anti-oxidation polyamide filament, which comprises the steps of preparation of organic-inorganic hybrid silicon dioxide aerogel, adsorption, preparation of procyanidine functional particles and melt spinning. According to the preparation method, the silicon dioxide aerogel is subjected to hybrid modification, a vinyl ether structure in 2-chloroethyl vinyl ether and silicon hydroxyl are subjected to electrophilic addition to form Si-O-C bonds, the Si-O-C bonds and a Si-O-Si network jointly form a semi-interpenetrating network structure, and the organic-inorganic hybrid silicon dioxide aerogel which is good in mechanical property, compact in structure and good in dispersity is obtained. And the procyanidine is subjected to adsorption protection, so that the high-temperature loss of the procyanidine in the chinlon preparation process is reduced. The procyanidine antioxidant polyamide filament prepared by the method has excellent antibacterial and antioxidant properties, the antibacterial rates on staphylococcus aureus, escherichia coli and candida albicans are all greater than 95% after the procyanidine antioxidant polyamide filament is washed with water for 50 times, and the free radical scavenging rate is greater than 92%.

The invention belongs to the technical field of sewage treatment, and particularly relates to a device and a method for treating sewage containing halogenated organic pollutants. The electroreduction dehalogenation-electrooxidation mineralization coupled green and efficient treatment method for degrading halogenated organic pollutant-containing sewage comprises the following steps: connecting a cathode membrane and an anode membrane to an external power supply, under the driving of differential pressure, enabling the sewage to firstly flow through the cathode membrane, dehalogenating in a nanopore channel of the cathode membrane by utilizing direct electroreduction to cooperate with indirect electroreduction, and then removing the halogenated organic pollutant in the nanopore channel of the anode membrane. And enabling the effluent of the cathode membrane to pass through the anode membrane, and carrying out electrophilic addition oxidation in a nano pore channel of the anode membrane by utilizing direct oxidation and indirect oxidation, thereby completing efficient and green removal of the organic pollutants after dehalogenation.

The invention discloses a novel cyclic dihydric alcohol as well as a preparation method and application thereof, cyclohexanone is used as a raw material, a dialdehyde monomer is obtained through electrophilic addition, and then a dihydric alcohol monomer is prepared through reduction hydrogenation. The unique advantages of the cyclohexanone structure are fully played, a new way is opened up for application of cyclohexanone, the prepared dihydric alcohol can be used as a polymeric monomer for preparing a polyurethane material, and the tensile property of the prepared polyurethane material is excellent.

The present invention provides a di(5-mononitroisosorbide) sulfate compound, a preparation method thereof, and an electrolyte. The structural formula of the di(5-mononitroisosorbide) sulfate compound of the present invention is shown in Formula I. The preparation method of the di(5-mononitroisosorbide) sulfate compound comprises the steps of: subjecting 5-mononitroisosorbide and thionyl chloride to an electrophilic addition reaction in the presence of a first solvent and an acid-binding agent to obtain an intermediate; adding an oxidizing agent to oxidize the intermediate in the presence of a second solvent to obtain a product; and purifying and drying the product. The di(5-mononitroisosorbide) sulfate compound has a mononitroisosorbide structure and a sulfonate structure, can form a good protective film at the interface of the positive and negative electrode materials, and has a low internal resistance, which can improve the battery's service life and cycle performance. Therefore, it is an excellent lithium-ion battery electrolyte additive that can expand the application field of 5-mononitroisosorbide derivatives. Formula I.