20 results about "Iodine catalysis" patented technology

The invention provides a preparation method and application of an air-stable sulfide composite electrolyte, and the method comprises the following steps: S1, weighing an M source (M = Cd, Mn and Zn), P2S5 and S powder according to a ratio of 1: 1: 3, adding iodine for catalysis, carrying out heat preservation at 700-720 DEG C for 6-7 days, and carrying out K + insertion, Li + exchange and ultrasonic centrifugation to prepare a LiMyPS3 nanosheet dispersion liquid; s2, dissolving PEO and LiTFSI in acetonitrile to form a film, drying to obtain a pure PEO film, immersing the pure PEO film into a dopamine Tris buffer solution with the concentration of 2 mg / ml and the pH value of 8.5, oscillating for 12-24 hours in an oxygen environment, and washing and drying to obtain a PDA-coated PEO film; and S3, carrying out suction filtration on the LiMyPS3 dispersion liquid to obtain a self-supporting membrane, stacking according to the sequence of "PDA-coated PEO membrane-sulfide membrane-PDA-coated PEO membrane", carrying out isostatic pressing at 10-20 MPa, and then carrying out vertical cutting at 0 DEG C to obtain the 20-30 [mu] m composite membrane. The film has the advantages of good air stability, almost no loss of conductivity after 30 days, room temperature conductivity of 9.2-10.2 ms / cm, excellent interface bonding force and mechanical strength, and stable window of 4.3-4.5 V, is adaptive to a high-voltage positive electrode, and can be used for a high-energy-density solid-state lithium battery.

The invention relates to a dapagliflozin impurity and a preparation method thereof, 5-bromo-2-chlorobenzoic acid (IV) is used as a raw material, (5-bromo-2-chlorphenyl) (4-ethyoxyl phenyl) ketone (III) is prepared through chlorination and Friedel-Crafts acylation, (5-bromo-2-chlorphenyl) (4-ethyoxyl phenyl) methanol (II) is obtained through reduction, and the benzhydryl ether impurity (I) is obtained through condensation under the catalysis of iodine. The preparation method has the advantages of simple operation, low cost, easily available raw materials and good product purity.

The invention relates to the technical field of preparation of chemical raw materials, in particular to a preparation process of tetrachlorophthalic anhydride, which comprises the following steps: S1, adding phthalic anhydride, chlorine, chlorosulfonic acid and a modified iodine catalyst into a reaction kettle for chlorination reaction to obtain a reacted material; and S2, transferring the reacted material into a crystallization kettle, carrying out cooling crystallization, introducing compressed air to recover chlorosulfonic acid, and carrying out temperature-controlled washing, centrifugal dewatering and drying to obtain a tetrachlorophthalic anhydride product. According to the preparation process, the iodine loss rate can be remarkably reduced, the catalytic efficiency and the reaction selectivity are improved, and finally high-purity and high-yield tetrachlorophthalic anhydride is prepared.

The invention discloses a preparation method of a heterojunction modified C60 supported monatomic iodine catalyst, and belongs to the technical field of nano materials and catalysis. According to the method, iodine atoms are stably loaded on a C60 carrier through oxidation pretreatment, heterostructure construction and a pyrolysis anchoring process. The method comprises the following steps: firstly, carrying out surface carboxylation activation on C60 by adopting nitric acid / sulfuric acid mixed acid; then mixing with thiourea, and performing high-temperature annealing to realize nitrogen-sulfur co-doping, so as to form a donor-acceptor pair heterojunction in a C60 skeleton; and finally, ball-milling and mixing with ammonium iodide or potassium iodate, and pyrolyzing in an inert atmosphere, so that iodine atoms and defect sites of the carrier form a C-I-N or C-I-S coordination structure, and monatomic-scale dispersion is realized. Topological defect anchoring points are created in C60 through heterojunction engineering, so that the iodine loading capacity reaches 5.0 wt% or above, the cycling stability is remarkably improved, the electron structure is optimized through nitrogen and sulfur synergistic doping, the half-wave potential of the catalyst in the oxygen reduction reaction reaches 0.85 V or above, and the apparent rate constant of persulfate for activating and degrading pollutants reaches 0.45 min <-1 >. The method has the advantages of simple process and low raw material cost, and is suitable for preparing efficient non-metal catalysts in the fields of fuel cells, metal-air battery electrodes, advanced oxidation water treatment and the like.

The present invention discloses a chiral aryl iodide catalyst using threonine as a chiral source, its synthesis method and application. The structural formula of the chiral aryl iodide catalyst is shown in Formula (12) or Formula (14), wherein R 1 is selected from a silyl protecting group, and R 2 is selected from methyl, trifluoromethyl, methyl ester or ethyl ester; R 3 is selected from acetyl, trifluoroacetyl, trichloroacetyl, tert-butylacetyl, benzoyl, substituted benzoyl, and the substituent on the substituted phenyl is mono-substituted or multi-substituted, and the substituent is methyl, methoxy, trifluoromethyl, trifluoromethoxy, ethyl, isopropyl, tert-butyl, halogen or nitro; R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 and R 11 each independently is selected from an alkane, a phenyl group or a substituted phenyl group, and the substituent is methyl, methoxy, trifluoromethyl, trifluoromethoxy, ethyl, isopropyl, tert-butyl, halogen or nitro; The catalyst of the present invention has the advantages of high enantioselectivity, low price and low toxicity in asymmetric organic catalysis.

The invention discloses a method for preparing delta-damascone by using an iodine catalyst, and belongs to the technical field of flavors and fragrances. Comprising the following steps: taking 1, 3-pentadiene and isopropylidene acetone which are cheap and easy to obtain as raw materials, taking iodine as a catalyst, performing D-A reaction to synthesize 4-acetyl-3, 5, 5-trimethyl cyclohexene, and condensing the 4-acetyl-3, 5, 5-trimethyl cyclohexene and ethyl acetate in the presence of a basic catalyst to obtain 1-(2, 6, 6-trimethyl-3-cyclohexene-yl)-1, 3-butanedione; according to the present invention, the iodine catalyst is adopted to replace the traditional Lewis acid catalyst, such that the waste acid water caused by the Lewis acid post-treatment is reduced, and the method has characteristics of simple operation, safety and environmental protection. In addition, the reaction is carried out under relatively mild conditions, so that the dangerousness of the reaction process is reduced, and industrial production is easy to realize.

The invention is suitable for the technical field of material chemistry, and provides a preparation method and application of a porous carbon-based iodine-rich catalyst. The preparation method comprises the following steps: uniformly mixing porous carbon with a compound containing an iodine element to obtain a suspension; placing the suspension in a reactor for reaction to obtain iodine-rich adsorption porous carbon; and cooling, cleaning and drying the iodine-enriched adsorbed porous carbon to obtain the porous carbon-based iodine-enriched catalyst. The iodine-doped porous carbon material, namely the porous carbon-based iodine-rich catalyst, is successfully prepared by reacting porous carbon with a compound containing an iodine element under a high-temperature condition. The method is conventional in equipment, simple to operate, low in cost and suitable for industrial production. The prepared porous carbon-based iodine-rich catalyst has mutually communicated porous structures and abundant surface microstructures. Performance tests show that the catalyst shows excellent catalytic activity, rapid dynamic property and good stability in water electrolysis hydrogen production, and has high application potential.

The invention belongs to the technical field of hydrogen production, and discloses a method and a device for coupling membrane-free water electrolysis hydrogen production with a zinc-iodine battery, firstly, a hydrogen evolution catalytic electrode, an iodine catalytic electrode and a zinc electrode are arranged in an electrolytic bath, the three electrodes are mutually independent in physical space, a set amount of iodine ion-containing I-electrolyte is injected into the electrolytic bath, and a set amount of iodine ion-containing I-electrolyte is injected into the electrolytic bath; the hydrogen evolution catalytic electrode is communicated with a cathode of an external power supply, the iodine catalytic electrode is communicated with an anode, then the external power supply is turned on, the iodine ion-containing I <-> electrolyte is stirred, electrolytic hydrogen production is carried out, then the external power supply is turned off, an external electric device or an electric storage device is connected with the iodine catalytic electrode and the zinc electrode, and a zinc-iodine primary battery reaction is carried out; zn < 2 + > precipitates in an alkaline environment, precipitates are cleaned regularly, and the zinc electrode is replaced. The invention further provides a device for implementing the method. The method and the device can solve the problems that an existing water electrolysis hydrogen production method is low in efficiency, a hydrogen production system is high in energy consumption, and oxygen evolution exists.

The invention relates to the production of methanol via the partial oxidation of methane using iodine(III) catalysts, which allow the reaction to be performed at low temperatures and pressures. Similar chemistry can be used to make methyl bisulfate from methane in the presence of oleum, and to make ethylene glycol via the partial oxidation of ethane.

The present invention discloses a method for preparing a graphene-enhanced copper composite material, and belongs to the technical field of composite material preparation. The present invention adopts highly active carbon quantum dots, which are dissolved, ultrasonicated, and activated in a solution, and iodine tincture and copper powder are added and stirred evenly, and freeze-dried to uniformly adsorb the carbon source and nucleation sites on the surface of the copper powder with a complex microstructure. Graphene is then grown in situ at a low temperature by iodine catalysis to prepare a well-coated, uniformly structured, and tightly bonded graphene / copper composite powder. Graphene-enhanced copper composite materials with a continuous structure and strong interface bonding are then prepared by sintering. The large specific surface area graphene coated evenly is utilized to improve the carrier and load transfer capacity of the composite material, which is beneficial to the transmission of electricity, heat, and force, so that the electrical conductivity of the composite material is as high as 90-100.8% IACS, the tensile strength reaches 207-263 MPa, and the thermal diffusion coefficient reaches 101.8-120.8 mm 2 / s, and its comprehensive performance is better than that of pure copper. In addition, the method is simple in process and easy to produce.

The present application relates to the field of heterocyclic synthesis and the field of organic photocatalysis, in particular to a preparation method and application of pyrrolo [3,4-c] pyrrole-1,3(2H,5H)-dione derivatives. The present application realizes one-step synthesis of a new photocatalyst, pyrrolo [3,4-c] pyrrole-1,3(2H,5H)-dione derivatives, from tetrahydroisoquinoline and methylene succinimide compounds under catalysis of elemental iodine in an air atmosphere. The technical scheme has the following advantages: (1) the required reagent is stable in nature, does not need pretreatment, is cheap and easy to obtain; (2) one-pot synthesis, obvious economic advantage in steps, no need for water-free and oxygen-free operation, time and labor saving; (3) the molecule itself does not contain metal elements, and no transition metal catalyst is needed, which fundamentally eliminates the problem of metal residues; (4) the use of cheap elemental iodine catalysis reduces environmental pollution and saves reaction cost; (5) the series of derivatives all have suitable oxidation-reduction potentials, and can be used as photocatalysts to catalyze multiple reactions; (5) as a catalyst, the catalytic efficiency is high, and only 0.5-1% loading is needed to catalyze the reaction.

The application discloses a preparation method of bis(2,3-cyclopropyl sulfide) disulfide and belongs to the technical field of organic synthesis. Epoxy chloropropane is reacted with thioacetate to obtain 2-(acetyl thiomethyl) oxirane; then, the acetyl group is removed by reaction with hydrochloric acid; then, the 2-(acetyl thiomethyl) oxirane is reacted with hydrogen peroxide under the catalysis of iodine or is reacted with sulfur powder and sodium hydroxide; finally, the 2-(acetyl thiomethyl) oxirane is reacted with thiourea to obtain bis(2,3-cyclopropyl sulfide) disulfide. In the application, chloroepoxy propane is used as a raw material, and intermediates in the whole reaction process can be purified, the purity of the final product is high, the obtained product can be used for high refractive index resin lenses (refractive index is greater than or equal to 1.70) and high-temperature-resistant optical coatings, and the product meets the requirements of the electronic and medical fields.

The present invention discloses a CABC-type asymmetric block copolymer and a preparation method thereof. The in-situ bromine-iodine conversion of a bromine initiator containing double initiation sites and an iodine agent generates a carbon-iodine bond active site, thereby initiating monomers for reversible complex-mediated polymerization. The first monomer is photo-initiated for polymerization through the carbon-iodine bonds at both ends, the second monomer is photo-initiated for chain extension polymerization through the carbon-iodine bonds at both ends, and the third monomer is thermally initiated for polymerization by the carbon-iodine bonds at both ends and the middle azo group simultaneously, finally obtaining a CABC-type asymmetric block copolymer. It overcomes the problems of cumbersome process and unstable controllability in the synthesis of CABC-type asymmetric block copolymers by traditional sequential polymerization, and solves the problems of difficult preparation and storage of iodine catalysts in the reversible complex-mediated polymerization system and easy thermal cleavage of end groups.

The present invention is applicable to the field of material chemistry technology, and provides a preparation method and application of a porous carbon-based iodine-rich catalyst. The preparation method comprises the following steps: uniformly mixing porous carbon with a compound containing iodine element to obtain a suspension; placing the suspension in a reactor for reaction to obtain iodine-rich porous carbon; cooling, washing and drying the iodine-rich porous carbon to obtain a porous carbon-based iodine-rich catalyst. The present invention successfully prepares iodine-doped porous carbon materials, i.e., porous carbon-based iodine-rich catalysts, by reacting porous carbon with a compound containing iodine element under high temperature conditions. The method has conventional equipment, simple operation, low cost, and is suitable for industrial production. The prepared porous carbon-based iodine-rich catalyst has an interconnected porous structure and rich surface microstructure. Performance tests show that the catalyst exhibits excellent catalytic activity, rapid kinetic properties and good stability in hydrogen production by electrolysis of water, and has high application potential.

The application discloses an isobenzofuranone compound, a preparation method and application thereof. The structural formula of the isobenzofuranone compound is shown as formula (I), wherein R 1 ~R 4 are respectively selected from C1-C6 alkyl, hydrogen, halogen or methoxy; R 5 is selected from C1-C6 alkyl, aryl or halogenated aryl. The application discloses a new compound with anti-pancreatic cancer activity, which has great drug research and development potential and can be used as a lead compound for the development of anti-pancreatic cancer drugs. The isobenzofuranone compound is synthesized by using a non-metal oxidant high-valence iodine catalyst, without using expensive metal catalysts, and meets the requirements of green chemistry. The isobenzofuranone compound has high biological activity, small toxicity and high selectivity, is a new compound which is not easy to be drug-resistant, and can effectively inhibit the proliferation of pancreatic cancer cells.

The invention relates to a preparation method of apixaban, which comprises the following steps: carrying out aldol condensation on ethyl methoxyacetate serving as a raw material and ethyl pyruvate to obtain an intermediate II, carrying out alkylation reaction on the intermediate II and 1, 2-dichloroethane to obtain an intermediate III, carrying out pyrazole synthesis reaction on the intermediate III and 4-methoxyphenylhydrazine to obtain an intermediate IV, carrying out alkylation reaction on the intermediate IV and 4-nitroaniline to obtain an intermediate V, and carrying out recrystallization on the intermediate V to obtain the apixaban. The preparation method comprises the following steps: carrying out ester group hydrolysis to prepare an intermediate VI, carrying out molecular lactamization in the presence of a condensing agent to prepare an intermediate VII, carrying out nitro reduction to prepare an intermediate VIII, carrying out amidation on the intermediate VIII and 5-bromovaleryl chloride under the action of an acid-binding agent, further carrying out an intramolecular alkylation reaction under the action of a strong alkali to prepare an intermediate IX, adding tert-butyl hydroperoxide and ammonia water, and carrying out a reaction under the action of a strong alkali to prepare the intermediate IX. Under the catalysis of iodine, carrying out oxidation amidation to prepare apixaban; the method has the advantages of cheap and easily available raw materials, easy realization of industrialization, high product purity, no dangerous process, simple equipment, novel route and short synthesis route.

The present invention discloses a method for preparing a chiral spirosteroid compound by using a chiral aryl iodide catalyst derived from chloramphenicol. The method comprises the following steps: adding a naphthol derivative to an organic solvent; sequentially adding an additive, a chiral aryl iodide catalyst, and an oxidant at an appropriate temperature to carry out a reaction; quenching the reaction with a quencher to obtain a product; and finally recovering the catalyst. The reaction process includes the following steps: reaction 1: #imgabs0# reaction 2: #imgabs1# reaction 3: #imgabs2# H on the benzene ring is replaced by a substituent R 1 , R 2 , R 3 , R 4 and R 5 Substituted or unsubstituted, when substituted R 1 , R 2 are each independently selected from alkyl, halogen, phenyl, alkyl acyl or phenyl acyl; R 3 is selected from halogen or alkoxy; R 4 and R 5 The present invention has mild reaction conditions, cheap and readily available raw materials, good catalyst catalytic effect, high product stereoselectivity, simple reaction operation, high yield, economical and practical, and environmentally friendly.

The application relates to the technical field, in particular to an improved preparation process of a JAK inhibitor (Molinitin), which is prepared from benzyl methyl ether as a starting material through five steps, and the specific steps are as follows: in the first step, benzyl methyl ether and acetic anhydride are subjected to a Friedel-Crafts acylation reaction under the catalysis of aluminum chloride to prepare an intermediate 2; in the second step, 4-acetyl benzyl methyl ether and aminoacetonitrile are subjected to one-pot oxidation through TBHP under the catalysis of iodine to prepare an intermediate 3; in the third step, N-(cyanomethyl)-4-acetyl benzamide is subjected to condensation through reflux reaction in pyridine and DMF-DMA to prepare an intermediate 4; in the fourth step, N-(cyanomethyl)-4-(3-(N,N-dimethyl)acryloyl) benzamide is subjected to condensation with guanidine hydrochloride under alkaline conditions to prepare an intermediate 5; and in the fifth step, N-(cyanomethyl)-4-(2-aminopyrimidin-4-yl) benzamide is subjected to Ullmann coupling reaction with 4-(4-bromophenyl)morpholine under the catalysis of copper glycinate to prepare Molinitin.

The invention relates to the production of [11C]CH3OSO2CF3, [13C]CH3OSO2CF3, [11C]CH3N(SO2CF3)2 or [13C]CH3N(SO2CF3)2 comprising reacting [11C]CH4 or [13C]CH4 with an iodine(III) catalyst. The 11C labelled products can be used to prepare radiotracer compounds containing an [11C]CH3 group for use in PET imaging.