17 results about "Propyl bromide" patented technology

The invention discloses a method for preparing isopentenyl indole alkaloid Debromolustramine B. The isopentenyl indole alkaloid Debromolustramine B belongs to the technical field of organic synthesis, an o-bromo aniline aldehyde compound is used as an initial raw material, and on the basis of novel chiral p-toluene sulfinyl guidance, cheap copper catalysis amido alpha-position arylation and 3, 3-dimethyl allyl bromide cyclization reaction, the isopentenyl indole alkaloid Debromolustramine B is synthesized, and the isopentenyl indole alkaloid Debromolustramine B is obtained. According to the present invention, the key aryl quaternary carbon chiral center in the isopentenyl indole alkaloid Debomolustramine B is constructed, and the isopentenyl indole alkaloid Debomolustramine B with the butyrylcholine esterase inhibition activity is prepared through the subsequent series of chemical conversion, such that the material basis is provided for the further research of the natural product Debomolustramine B and the analogue thereof. The method has the advantages that the reaction conditions are mild, the cheap metal copper is used as the catalyst, the synthesis route is short, the energy consumption is low, the environmental protection is facilitated, and the large-scale chiral preparation of the isopentenyl indole alkaloid Debromofloutramine B is facilitated; the method also has the characteristics of relatively good atom economy and high product yield.

The method for manufacturing an intermediate compound for shikonin synthesis of the present invention comprises the steps of: reacting 1,5-dihydroxynaphthalene with dimethyl sulfate to prepare 1,5-dimethoxynaphthalene; reacting 1,5-dimethoxynaphthalene with N-bromosuccinimide (NBS) to prepare 1,5-dibromo -4,8-dimethoxynaphthalene; introducing a methoxy group into 1,5-dibromo-4,8-dimethoxynaphthalene using copper iodide (CuI) and 1,10-phenanthroline as a catalyst to prepare 1,4,5,8-tetramethoxynaphthalene; performing formylation of 1,4,5,8-tetramethoxynaphthalene using phosphoryl chloride (POCl3) to prepare 2-formyl-1,4,5,8-tetramethoxynaphthalene; and forming a boron complex using pinacolborane (HBpin) and 3,3-dimethylallyl bromide and reacting the boron complex with 2-formyl -1,4,5,8-tetramethoxynaphthalene to prepare a prenylated shikonin intermediate. Compared to conventional synthetic methods, the method of the present invention offers milder reaction conditions, shorter reaction time, and improved yield, thereby greatly enhancing the economic feasibility of shikonin synthesis.

The invention belongs to the field of high polymer materials, and relates to a clean construction method of a halogen-free phosphorus-free flame-retardant epoxy polymerization system. The preparation method comprises the following steps: preparing an intermediate I from 2, 2 '-diallyl bisphenol and allyl bromide under the action of potassium carbonate; carrying out rearrangement reaction on the intermediate I to prepare an intermediate II; and carrying out etherification and ring-closure reaction on the intermediate II and epoxy chloropropane under the action of a catalyst and sodium hydroxide to obtain the epoxy resin monomer III. The halogen-free phosphorus-free flame-retardant epoxy resin polymer is obtained by mixing an epoxy resin monomer with a curing agent, melting, performing injection molding and curing. The halogen-free and phosphorus-free flame retardant polymer obtained by the invention can reach the flame retardant grade of UL94-V0 grade.

This invention provides a ( E This invention relates to the field of pharmaceutical synthesis technology and provides a method for synthesizing 3,5-dihydroxy-4-isopropylstilbene. The method comprises three steps: starting with 3,5-dimethoxy-bromobenzene as a starting material, isopropylation is carried out under acidic conditions to obtain 3,5-dimethoxy-4-isopropylstilbene; further, a Heck reaction is performed with styrene under palladium catalysis to obtain (…). E )-3,5-dimethoxy-4-isopropylstilbene; demethylation reaction yields the ( E 3,5-Dihydroxy-4-isopropylstilbene. Compared to existing synthetic routes, the synthetic method of this invention significantly shortens the synthetic path, has higher atom utilization, higher product yield, and is environmentally friendly.

The invention discloses a modified molecular sieve capable of adsorbing and regenerating high-boiling-point substances and a preparation method thereof. According to the molecular sieve, a tetrapropylammonium bromide and N-bromoacetamide double-template system is adopted, a high-silicon ZSM-5 molecular sieve with the silica-alumina ratio larger than 300 is prepared through a guided gel-assisted hydrothermal synthesis method, and Ni metal is loaded for modification. The product has excellent hydrophobicity (the water contact angle is greater than 120 degrees) and a mesoporous structure, and can efficiently adsorb macromolecular organic matters such as coal tar and the like. Ni2 + / NiO bifunctional sites are innovatively introduced, adsorption selectivity is enhanced through pi-complexation, low-temperature desorption assisted by ethanol at the temperature of 80-120 DEG C is realized, and the desorption rate is increased by 3-5 times. Compared with a traditional method, the technology has the advantages of cheap raw materials, high crystallinity (greater than 95%), carbon deposition resistance, cyclic regeneration and the like, and is suitable for resourceful treatment of high-boiling-point organic matters in industrial waste gas.

An electrolyte (102) of a zinc-bromine static battery (104), comprising zinc bromide in molar concentration from 1.5 to 3.0 M; a mixture of two or more quaternary ammonium salts in 30 to 55 % of the molar concentration of the ZnBr2; a glycol based anti-freezing agent in molar concentration 0.1 to 2.0 M; and one or more additional supporting ionic conducting agents selected from zinc chloride, potassium chloride, magnesium chloride, lithium chloride and calcium chloride, where each or the combination are present in a molar concentration 0.5 to 2 M. The ammonium salts may be selected from tetrapropylammonium bromide (TPAB) or chloride or tetrabutylammonium bromide (TBAB) or chloride along with tetraethylammonium bromide (TEAB) or chloride. The anti-freezing agent may be selected from monoethylene glycol, propylene glycol, 1,3-butylene glycol, polyethylene glycol 200, polyethylene glycol 400, or a combination thereof. The electrolyte may be free of pH maintaining agents and buffering agents.

The invention provides a preparation method of octabromoS ether, and belongs to the technical field of flame-retardant materials. According to the preparation method, bisphenol S and allyl bromide are subjected to a carbon-oxygen coupling reaction under catalysis of a transition metal compound catalyst, bisphenol S diallyl ether and hydrogen bromide are obtained, hydrogen bromide can be recycled in a subsequent addition reaction, and the cost is saved; then hydrobromic acid and bisphenol S diallyl ether are subjected to an addition-electrophilic substitution reaction under catalytic oxidation of hydrogen peroxide to obtain octabromo-S ether, and high-toxicity bromine is not adopted; hydrogen peroxide is reduced into water in the reaction, so that the method is green and environment-friendly.

This invention provides a ZSM-48 and ZSM-5 composite molecular sieve, its preparation method, and its application. The method includes: mixing a template agent, a silicon source, an aluminum source, water, and an alkali source in a molar ratio of (0.01-0.5):1:(0.005-0.05):(10-100):(0.03-0.2) to obtain an initial gel; the template agent is tetrapropylammonium bromide and / or hexamethyldiammonium bromide; adding seed crystals to the initial gel and crystallizing to obtain a crystallized product; the seed crystals are ZSM-5 molecular sieve and / or ZSM-48 molecular sieve, with a mass ratio of seed crystal to silicon source of (0.01-0.2):1; calcining and ammonium exchange of the crystallized product to obtain the ZSM-48 and ZSM-5 composite molecular sieve. This invention significantly improves product purity and inhibits the formation of impurity crystals while ensuring the relative crystallinity of the composite molecular sieve by introducing heterogeneous seed crystals and a two-step crystallization process.

The invention provides a preparation method of spirolactone, and relates to the technical field of organic synthesis. The preparation method of spirolactone provided by the invention comprises the following steps: taking 4-androstene-3, 17-diketone as a raw material, carrying out nucleophilic addition reaction on the 4-androstene-3, 17-diketone and an organic zinc reagent 3-tert-butoxy-3-oxypropyl zinc bromide, then carrying out elimination-lactonization under the catalysis of trifluoroacetic acid, and completing lactonization while removing tert-butyl; then sequentially carrying out etherification reaction and oxidative dehydrogenation reaction to obtain canrenone, and finally carrying out addition reaction on canrenone and thioacetic acid to obtain spirolactone. The preparation method provided by the invention provides a novel construction method of 21-carboxylic acid-gamma-lactone, the method is good in specificity, the total mass yield of spirolactone is greater than 92%, and the total mass yield is high; moreover, the HPLC purity of the spirolactone prepared by the preparation method provided by the invention is greater than 99.7%, which is far higher than the purity of the spirolactone prepared by the existing process.

The invention belongs to the technical field of fine chemicals, medicines and materials, and particularly relates to a preparation method of an aryl triepoxypropane compound. The preparation method comprises the following steps: 1) mixing 2, 6-diallylphenol with a first solvent, adding allyl bromide and alkali to obtain a mixture, heating and refluxing the mixture, reacting, and cooling to room temperature to obtain 1, 3-diallyl-2-allyloxybenzene as shown in a formula I; and 2) reacting the 1, 3-diallyl-2-allyloxybenzene as shown in the formula I, a metal complex catalyst and an oxidizing agent in a second solvent to obtain the aryl triepoxypropane compound as shown in a formula II. The preparation method has the advantages of cheap and easily available raw materials, simple and mild reaction, low catalyst price and high reaction yield, and can realize industrial production.

The application relates to the technical field of high polymer materials, and discloses a single-end type dihydroxyalkylamine modified polysiloxane as well as a preparation method and application thereof, and the structure is shown in formula I, wherein the value range of n is a natural number of 10-65. The preparation process is as follows: diethanolamine, hexamethyldisilazane, allyl bromide and alpha-(trimethylsilyl)-omega-dimethylsilyl polydimethylsiloxane shown in formula M1 are used as raw materials, and a single-end trimethylsilyl group and a dihydroxyalkylamine group are substituted at the other end under the catalysis of a Karstedt catalyst, the dihydroxyalkylamine modified polysiloxane has excellent stability and hydrophilicity, and the emulsion prepared by using the dihydroxyalkylamine modified polysiloxane has high hydrophilicity and good yellowing resistance when treating fabric.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of 2-(4-(cyclopropyl formyl) phenyl)-2-methyl tert-butyl propionate 13C. Comprising the following steps: introducing carbon dioxide (13C) into tetrahydrofuran and a reagent A at-80 DEG C to synthesize cyclopropanecarboxylic acid (13C), wherein the reagent A is cyclopropyl magnesium bromide and cyclopropyl magnesium iodide: adding the cyclopropanecarboxylic acid (13C), dichloromethane, dimethyl hydroxylamine hydrochloride and 4-dimethylaminopyridine into triethylamine at room temperature, and reacting at the temperature of-80 DEG C to obtain the cyclopropanecarboxylic acid (13C). The preparation method comprises the following steps: synthesizing N-methoxy-N-methyl cyclopropanecarboxamide-13C from 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride; the preparation method comprises the following steps: adding 2-(4-bromophenyl)-2-tert-butyl methyl propionate and tetrahydrofuran into a reaction kettle, dropwise adding an alkali solution at the temperature of-40 DEG C, and dropwise adding N-methoxy-N-methylcyclopropanecarboxamide-13C to synthesize 2-(4-(cyclopropanecarboxyl) phenyl)-2-tert-butyl methyl propionate-13C, thereby obtaining the 2-(4-(cyclopropanecarboxyl) phenyl)-2-tert-butyl methyl propionate-13C. The method is reasonable in route, low in cost, high in yield and easy to industrialize.

The invention belongs to the technical field of molecular sieve synthesis, and discloses a preparation method of a flaky hollow TS-1 molecular sieve for phenol hydroxylation, the molecular sieve and application, and the preparation method comprises the following synthesis steps: dropwise adding tetraethyl orthosilicate into an aqueous solution containing tetrapropylammonium hydroxide; after clarification, dropwise adding a solution containing tetrabutyl titanate and isopropanol into the solution; after high-temperature alcohol removal, N, N-dimethylformamide is added; carrying out hydrothermal crystallization, centrifugation, drying and calcination; adding the collected maternal zeolite into an aqueous solution of tetrapropylammonium bromide and ethanolamine; and carrying out hydrothermal crystallization, centrifugation, drying and calcination. The method is low in cost and simple to operate, the sheet-shaped hollow titanium silicalite molecular sieve is synthesized, the diffusion mass transfer rate is increased, and the sheet-shaped hollow titanium silicalite molecular sieve has a large number of hexa-coordination active titanium species and has good catalytic activity in 1-hexene epoxidation, cyclohexene epoxidation, propylene epoxidation and phenol hydroxylation reactions.

The application discloses a method for hydrogen sulfide resource utilization by using surfactant-induced modified zeolite to catalyze butene and hydrogen sulfide to synthesize butyl mercaptan. The surfactant-induced modified zeolite is prepared by the following steps: dissolving 0.3-0.4g of cetyl tripropyl ammonium bromide in 0.06-0.1mol / L of NaOH aqueous solution, then adding 1-1.2g of FAU type zeolite, stirring for 1-2h at room temperature, transferring the mixture into a high-pressure reaction kettle, heating for 30-90h at 150-170 DEG C, performing solid-liquid separation, calcining the solid at 500-700 DEG C for 3-5h, and then using an equal-volume impregnation method to place the calcined solid in a molybdate solution, standing, and drying to obtain the surfactant-induced modified zeolite. The catalyst has the advantages of good stability, good sulfur resistance and high selectivity, and the service life of the catalyst is greatly improved.

The invention relates to the technical field of acidification and yield increase of petroleum and natural gas, and discloses a drag-reducing retarded acid solution composition, a drag-reducing retarded acid solution, and a preparation method and application of the drag-reducing retarded acid solution. The composition comprises the following components: a retarder which is compounded by at least two of C2-C8 binary acids; the corrosion inhibitor is at least one of pyridine quaternary ammonium salt, quinoline quaternary ammonium salt, naphthenic acid imidazoline and lauric acid imidazoline; the corrosion inhibition synergist is at least one of antimony trioxide, glutaraldehyde and potassium iodide; the drag reducer is prepared from at least one of acryloyloxyethyl trimethyl ammonium chloride, 2-methacryloyloxyethyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride and N-vinyl-2-pyrrolidone, and N, N-dimethyl dodecyl allyl ammonium bromide, N, N-dimethyl hexadecyl allyl ammonium bromide and N, N-dimethyl hexadecyl allyl ammonium bromide, and at least one of N, N-dimethyl hexadecyl allyl ammonium bromide and N, N-dimethyl hexadecyl allyl ammonium bromide. And polymerizing at least one of N, N-dimethyl octadecyl allyl ammonium bromide. The drag-reducing and retarding acid liquor can reduce the corrosion rate and corrosion to a tubular column under the condition of ultrahigh temperature.

The invention relates to the technical field of agricultural disease control, in particular to application of indole compounds and pharmaceutically acceptable salts, solvates, crystal forms, prodrugs, stereoisomers and tautomers thereof in preparation of drugs for inhibiting pathogenic fungi pathogenic key protein kinase CgSlt2. The invention provides a novel CgSlt2 targeting inhibitor for the first time, in particular, indole compounds ((S)-N-(1-(1H-indol-3-yl)-4-(methylamino)-4-oxobutyl-2-yl)-8-bromine-1, 6-naphthyridine-2-formamide) and ((S)-N-(2-((1H-indol-3-yl)-1-(methylamino)-1-oxopropyl)-8-bromine-1, 6-naphthyridine-2-formamide) are subjected to a one-pot reaction to prepare the CgSlt2 targeting inhibitor. The CgSlt2 inhibitor (2, 6-naphthyridine-2-formamide) has the characteristics of strong target property and high activity, and shows excellent pathogenicity for inhibiting colletotrichum gloeosporioides complex strains.

The present invention belongs to the technical field of lithium metal battery electrolytes and provides a low-volatility electrolyte suitable for high-temperature, high-capacity lithium batteries and a preparation method thereof. 1-Ethylimidazole is first prepared by an alkylation reaction of imidazole and ethyl bromide, and further reacted with 3,3,3-trifluoropropyl bromide and 2-chloroethanol methyl ether. The ionic liquid molecular design combines a trifluoro group with an ether structure. The introduction of the trifluoro group reduces the vapor pressure of the electrolyte, thereby suppressing volatility under high temperature conditions. The oxygen atoms in the ethanol methyl ether group react with metallic lithium to form a stable lithium alkoxide, which helps to form a dense and stable solid electrolyte interface film on the negative electrode surface. The sulfonic acid group can promote the formation of a high-quality solid electrolyte interface film on the negative electrode surface through strong interaction with lithium ions, thereby suppressing the growth of lithium dendrites. The phosphate group inhibits the decomposition of the electrolyte under high temperature conditions through its chemical stability.