31 results about "Cyclobutane" patented technology

The invention provides a preparation method of (S)-oxetane-2-methylamine. The preparation method of (S)-oxetane-2-methylamine comprises the following steps: (1) carrying out ring closing reaction on a compound A under an alkaline condition to obtain a compound B; (2) reacting the compound B with dibenzylamine to obtain a compound C; (3) reacting the compound C with a reducing agent to obtain a compound D; (4) reacting the compound D with paratoluensulfonyl chloride to obtain a compound E; (5) reacting the compound E with alkali to obtain a compound F; and (6) carrying out a reaction on the compound F and palladium on carbon to obtain the (S)-oxetane-2-methylamine. According to the preparation method provided by the invention, ring expansion reaction using trimethylsulfoxide iodide in the prior art is avoided, the problem that residual sulfur elements cause poisoning of a palladium-carbon catalyst is solved, meanwhile, sodium azide is also avoided, and the preparation method is safe and reliable in process, high in chiral purity and yield and suitable for industrial large-scale production.

Disclosed is a method for preparing oxetan-2-ylmethanamine, which belongs to the field of organic synthesis. [2-(1-ethoxyethoxy)methyl]propylene oxide is used as an initial raw material, and reacted in the presence of potassium tert-butoxide and trimethylsulfoxonium iodide; the resulting product is reacted with a sulfonyl compound and triethylamine; the resulting product is reacted with a compound of phthalimide; the resulting product is reacted with an amino group-containing compound, to obtain oxetan-2-ylmethanamine. The method according to the disclosure allows for an overall yield of not less than 30% in scale-up production (kilogram level), which is higher. Moreover, compared with the traditional method for preparing oxetan-2-ylmethanamine, a palladium-carbon catalytic hydrogenation step is not required, and dangerous chemical-sodium azide is not required in the method according to the disclosure. Thus, the method has high safety, low production cost, simple operations, and thereby is suitable for industrial production.

The present invention relates to compounds of formula (I) or formula (II) or pharmaceutically acceptable salt, solvate or hydrate thereof, wherein said compound of formula (I) and said compound of formula II each comprises at least one ONO2 or ONO moiety; R1 is C1-C3alkyl; R2 is H, C1-C6alkyl, C3-C6cycloalkyl, C1-C2alkoxy, C2-C4alkenyl; R3 is C1-C4alkyl optionally substituted with C1-C2alkoxy, C3-C4cycloalkyl, C2-C4alkenyl; R4 and R5 are each independently H or C1-C6alkyl optionally substituted with F, OH, ONO, ONO2, COOH, C1-C3alkoxy, C3-C6cycloalkyl; or together with the nitrogen atom to which they are attached form a heterocyclic ring, wherein preferably said heterocyclic ring is selected from aziridine, azetidine, pyrollidine, piperidine, morpholine, piperazine, homo-piperazine, 2,5-diazabicyclo[2,2,1]heptane and 3,7-diazabicyclo[3,3,0]octane, wherein said heterocyclic ring is optionally substituted with independently one or more R6; R6 is C1-C6alkyl optionally substituted with independently one or more halogen, OH, ONO, ONO2, C1-C3alkoxy, C1-C3haloalkoxy, COOR7, NR8R9, C═NR10; R7 is H, or C1-C4alkyl optionally substituted with F, OH, ONO, ONO2, NR8R9; R8 and R9 are independently H, or C1-C4alkyl optionally substituted with ONO, ONO2; R10 is C1-C4alkyl optionally substituted with F, ONO, ONO2; C3-C6cycloalkyl; pharmaceutical compositions thereof, and their use in methods of treating or preventing a disease alleviated by inhibition of PDE5 in a human or in a non-human mammal.

The invention relates to a method for synthesizing a 3, 3-dimethoxy cyclobutane-1, 1-isopropyl diformate compound IV, and the reaction is as follows: M is selected from potassium, sodium, lithium, calcium and magnesium; comprising the following steps: (1) carrying out salt forming reaction on a compound shown as a formula I in an organic solvent in the presence of alkali, and filtering after the reaction is completed to obtain a solid compound shown as a formula II; and (2) carrying out ring closing reaction on the solid compound as shown in the formula II and a compound as shown in a formula III in an aprotic solvent in the presence of a catalyst to obtain a compound as shown in a formula IV. The method is simple in synthesis route, mild in process condition, simple and convenient to operate, high in yield and good in product purity, solves the technical problems of tar impurities and alcohol ester exchange byproducts in the prior art, and is suitable for industrial large-scale production.

The invention relates to a synthesis method of chiral N-Fmoc-2-methyl azetidine-2-carboxylic acid, and relates to the technical field of organic synthesis.The synthesis method comprises the following steps that Fmoc-alpha-methyl-L-glutamic acid-5-tert-butyl ester is subjected to deprotection, and a compound I is obtained; carrying out esterification reaction on the compound I and aryl halide in an alkaline solution to obtain a compound II; removing an Fmoc protecting group from the compound II in an alkaline solution to obtain a compound III; the compound III is subjected to lactamization under the action of trimethylchlorosilane and tert-butyl magnesium bromide, and a compound IV is obtained; selectively reducing amide of the compound IV under the action of a borane reducing reagent to obtain a compound V; hydrolyzing the compound V in an alkaline solution, and removing benzyl to obtain a compound VI; and protecting the amino group of the compound VI through Fmoc to obtain a compound VII, namely the chiral N-Fmoc-2-methyl azetidine-2-carboxylic acid. The method has the effect of improving the synthesis efficiency of the chiral N-Fmoc-2-methyl azetidine-2-carboxylic acid, and the product has high yield and purity.

The present invention relates to a novel salt of an imidazo[1,2-a] pyridine compound, and more specifically, to azetidin-1-yl\{8-[(2,6-dimethylbenzyl)amino]-2,3-dimethylimidazo[1,2-a]pyridin-6-yl\}methanone diphosphate and a method for preparing same. The azetidin-1-yl\{8-[(2,6-dimethylbenzyl)amino]-2,3-dimethylimidazo[1,2-a]pyridin-6-yl\}methanone diphosphate according to the present invention has excellent solubility, volume density, light / temperature stability, acid / base stability, and the like, and thus can be usefully used in the formulation of pharmaceuticals.

The invention discloses a copper-catalyzed aryl aldehyde ortho-position direct C-H etherification method, which comprises the following steps: by taking aryl aldehyde as a raw material, adding alcohol or phenol as shown in a formula (II), a copper catalyst, a guiding group, alkali and a solvent into a reactor, and reacting in an argon gas atmosphere to prepare an aryl ether compound as shown in a formula (III), a substituent group R1 is hydrogen, methyl, trifluoromethyl, methoxyl, phenyl, iodo, isopropyl, trimethylsilyl, dimethylamino, fluoro, chlorine, ester, tourmaline, naphthyl, isoquinolyl, benzothienyl or phenanthryl; a substituent group R2 is hydrogen, methyl, trifluoromethyl, methoxyl, phenyl, iodo, isopropyl, trimethylsilyl, dimethylamino, fluoro, chlorine, ester, tourmaline, naphthyl, isoquinolyl, benzothienyl or phenanthryl; and a substituent group R2 is methyl, 4-fluorophenyl, cyclobutane methyl, 4-tert-butyl phenyl, pentafluorophenyl, 4-cyanophenyl, 4-methyl ester phenyl, 3-nitrophenyl, adamantane methyl, cyclohexyl or an oestrone analogue. The copper catalyst and amino acid which are low in cost and easy to obtain are used as guiding groups, the operation process is simple and efficient, and the corresponding aryl ether compound can be obtained with the good yield.

The invention belongs to the technical field of biological medicines, and particularly relates to a synthetic method and application of a cyclobutane and chroman skeleton molecular compound, which is a method for synthesizing a cyclobutane and chroman skeleton molecular compound through a triplet-triplet energy transfer mechanism by using a blue light excitation photocatalyst under a mild condition. The invention discloses a method for constructing a cyclobutane and chroman skeleton molecular compound by efficiently, highly regionally and stereoselectively catalyzing intramolecular [2 + 2] cycloaddition of a 2H-chromene compound, and further explores the application potential of the cyclobutane and chroman skeleton molecular compound in research and development of anti-glioma drugs. The obtained compound can specifically and effectively kill glioma stem cells, and a new lead compound and thought are provided for research and development of anti-glioma drugs.

The present application provides a kind of singlet oxygen activated photo-cage chemiluminescence molecule, which has the structure shown in formula (I), wherein X is hydrogen or halogen, PC represents photo-cage group, R 1 It is an electron-withdrawing group containing oxygen and / or nitrogen, R 2 It is selected from adamantane, cyclobutane, methyl cyclobutyl formate and tetrahydrothiopyran-1,1-dioxide. The chemiluminescence molecule is activated by singlet oxygen and triggered by light of a specific wavelength, and through the processes of oxidation, photolysis, electron transfer, etc., an excited state benzoate structure is generated, which emits blue-green light when returning to the ground state. 2 Group, photo-cage group and R 1 Electron-withdrawing group synergistic effect, oxidation, photolysis, electron transfer, etc. process, generate excited state benzoate structure, it emits blue-green light when returning to the ground state.

The present application relates to a kind of flame-retardant polyester solid electrolyte membrane and its preparation method, belong to solid battery technical field, the preparation raw material of flame-retardant polyester solid electrolyte membrane includes neopentyl glycol diacrylate, 1-methyl-1-propyl piperidine-1-ol double ((trifluoromethyl) sulfonyl) imidazole, fluorinated ethylene carbonate, cyclobutane sulfone, sodium bis (trifluoromethylsulfonyl) imide, triethylene glycol dimethyl acrylate, azobisdimethylvaleronitrile, dust cloth, and the flame-retardant performance of this flame-retardant polyester solid electrolyte membrane is excellent, while the performance of flame-retardant polyester solid electrolyte membrane in electrochemical window and ionic conductivity etc. Excellent, the assembled solid battery has excellent electrochemical performance and stability at room temperature, and can be adapted to a variety of positive electrode materials, it is beneficial to the commercialization development of solid battery.

This disclosure provides a method for treating sulfolane waste liquid, wherein the sulfolane waste liquid is mixed with a photocatalyst and then subjected to a dark reaction and a photocatalytic reaction sequentially; wherein the photocatalyst is a BiPO4 / C3N4 composite photocatalyst. This method is green, energy-saving, simple, and efficient, and can convert sulfolane in the sulfolane waste liquid into sulfolane and sulfuric acid under normal temperature and pressure conditions without the addition of external organic reagents. In this method, sulfolane is directly released in gaseous form, reducing the time and energy costs associated with waste liquid separation; small molecule organic pollutants in the sulfolane waste liquid are degraded under photocatalysis, leaving only the sulfuric acid generated in the reaction and a small amount of the original inorganic salts after degradation.

The invention relates to stoichiometric salts of tetracarboxylic acids and diamines of the general formula (I) wherein R1 is selected from the group consisting of tetravalent residues of butane, cyclobutane, cyclopentane, cyclohexane, tetrahydrofuran and benzophenone and R2 is selected from the group consisting of divalent residues of unbranched, branched or cyclic aliphatic hydrocarbons having 3 to 15 carbon atoms, with the proviso that the salts of the formula (I) are water-soluble and are selected from the group consisting of compounds (1) to (28); and to polyimides prepared from these salts by polycondensation.

The application discloses a method for synthesizing polyether sulfone resin, and specifically comprises the following steps: adding solvent cyclobutane sulfone into a reactor provided with a nitrogen gas pipe, a gas distributor, mechanical stirring and a water separation condensing device, starting stirring, and adding monomer 4,4'-dichlorodiphenyl sulfone, bisphenol S and a salifying agent; after nitrogen replacement, the nitrogen flow is adjusted, and the temperature is raised to 210-240 DEG C; the gas distributor is used for distributing nitrogen, the system is continuously bubbled by nitrogen flow for dehydration, and the reaction is carried out for 3-5 hours; the nitrogen is turned off, the polymerized mucus is poured into water for precipitation, and the polyether sulfone resin is obtained through the steps of crushing, washing and drying. The application uses high-purity nitrogen flow for dehydration, thus avoiding the addition of flammable and toxic organic water-carrying agents, improving operation safety, not polluting products, and being simple in operation and short in reaction period.

This invention provides a method for synthesizing milobalin benzylsulfonic acid, comprising the following steps: a chiral enone undergoes a condensation reaction with cyanoacetate in the presence of ammonium acetate to obtain an unsaturated cyano ester; next, the unsaturated cyano ester undergoes a condensation reaction with nitromethane to obtain a nitro ester; the nitro ester is then deesterified at high temperature to obtain a chiral nitro nitrile, which is then reduced to a chiral amino nitrile; subsequently, the chiral amino nitrile is hydrolyzed to obtain the free base of milobalin; finally, the free base of milobalin is salted with benzylsulfonic acid to obtain milobalin benzylsulfonic acid. This invention stereospecifically constructs a chiral cyclobutane quaternary carbon center to obtain a chiral nitro ester with a single stereoconfiguration, avoiding the chiral isomer waste generated by chiral isomer resolution, eliminating the need for chiral column separation or chiral resolution, significantly reducing production costs, and simultaneously avoiding the environmental pollution caused by residual heavy metal titanium in the product and solid waste heavy metal titanium.

To provide a composition capable of giving a cured product exhibiting a high refractive index and having good film-forming properties.SOLUTION: The composition contains a compound (A) having a thiirane group or a thietane group, and a compound (B) having a group represented by formula (b) and a urethane bond in the molecule. [In Formula (b), * represents a bonding position. ] SELECTED DRAWING: None

Described is a process for preparing a recycle content polyester, the process comprising obtaining a recycled propylene composition derived from cracking a recycle content pyrolysis oil composition made from a waste plastic-containing stream, using the recycled propylene as a feedstock in a reaction scheme to produce a polyester reactant, and reacting the polyester reactant to prepare at least one polyester.

The invention relates to the technical field of analytical chemistry mass spectrum imaging, in particular to a P-B reaction online detection system and method, and the system comprises a sample fixing unit, a multi-dimensional control platform, a fluid transmission unit, an auxiliary catalysis unit and a mass spectrum acquisition unit. According to the present invention, the P-B reaction and the mass spectrometry imaging technology are combined, the P-B reaction is adopted to generate the oxetane structure at the double bond through the ultraviolet light induced [2 + 2] cycloaddition reaction, and the characteristic fragment is generated after the collision induced dissociation so as to achieve the accurate positioning of the double bond position, and solve the problem of the lipid isomer spatial distribution analysis; meanwhile, accurate positioning and analysis of lipid carbon-carbon double bond positions in a complex biological sample are realized by utilizing high sensitivity and spatial resolution capability of a mass spectrum imaging technology; the method can be applied to the fields of biomedical research, metabonomics and drug development, and an innovative analysis method is provided for lipid molecular structure analysis and function research.

A method is for synthesizing an oxetane compound by a microreactor. The synthesis method includes: introducing trimethylolpropane and carbonate into the microreactor in the presence of an alkaline catalyst, and synthesizing the oxetane compound by means of a micro-reaction continuous flow process under an inert solvent or a solvent-free condition. Compared with conventional reactors, the microreactor has the advantages of being high in heat transfer mass transfer coefficient, good in mixing performance, easy to control in temperature, safe and controllable in process. The three oxetane products are produced by utilizing the advantages of the microreactor, thereby greatly improving the mass transfer heat transfer performance of a reaction system, shortening the reaction time, improving the production efficiency, particularly avoiding the long-time high-temperature process in the pyrolysis process, reducing the production of high-boiling-point by-products, improving the yield, realizing continuity and automation of the process, and improving process safety.

This invention belongs to the field of photobiological chiral catalytic synthesis, and relates to an artificial photoenzyme, its preparation, and its application in photobiological chiral catalytic synthesis. This artificial photoenzyme is constructed by inserting an organic photosensitizer into a natural protein backbone using site-directed protein chemical modification technology. It can catalyze a [2+2] asymmetric photocycloaddition reaction of a 2-functionalized alkenylindole derivative under visible light to generate a chiral cyclobutane-fused tetracyclic indole spirocyclic compound. The artificial photoenzyme provided by this invention, constructed using site-directed protein chemical modification, can achieve highly efficient asymmetric photocatalytic reactions through energy transfer pathways, and features green environmental protection, mild conditions, and high reactivity.

The invention relates to the technical field of organic synthesis, in particular to a sulfolane spirofluorene compound and a preparation method thereof.The sulfolane spirofluorene compound has the structure shown in the formula (1), the preparation method provided by the invention has the advantages of high reaction activity, mild catalytic reaction conditions, high yield of the target compound, simple post-treatment, no metal pollution, accordance with green chemistry concept and the like. Formula (1).

The application relates to a continuous flow preparation process of cyclobutane tetracarboxylic dianhydride, maleic anhydride is added into a material storage bottle, a reaction solvent is added, the saturated solution of maleic anhydride is prepared by fully stirring, and temperature control is conducted on the saturated solution; the light source of a reactor is turned on in advance, the saturated solution of maleic anhydride is sent to the reactor, the reaction liquid output from the reactor is sent to a product separator, the separated solid is recycled, and the liquid is sent back to the material storage bottle; a circulating channel is formed among the material storage bottle, the reactor, the product separator and the material storage bottle, and the circulating channel is always maintained in a fluid flow state. The application constructs the continuous flow production equipment capable of always maintaining the fluid flow, the solid separated in the reactor by light excitation can be timely taken into the product separator for separation, the solid cannot adhere to the inner wall of the reactor to affect the light blocking, and the light can always be more uniformly and thoroughly penetrated through the reactor and utilized.

The present invention addresses the problem of providing a composition which can yield a cured product that exhibits a high refractive index and high adhesion, and which has excellent film-forming properties.　The present invention provides a composition containing a compound (A) that has a thiirane group or a thietane group, and a compound (B) that is represented by formula (B). [In formula (B), x, y, and z represent 1-5.　Rx, Ry, and Rz each represent a monovalent hydrocarbon group. When there are multiple Rx, Ry, and Rz, the multiple Rx, Ry, and Rz may be the same or different.　bx, by, and bz represent 0-4, the sum of x and bx is 5 or less, the sum of y and by is 5 or less, and the sum of z and bz is 5 or less.　Rbx, Rby, and Rbz each represent a monovalent substituent. When there are multiple Rbx, Rby, and Rbz, the multiple Rbx, Rby, and Rbz may be the same or different.]

The invention discloses a degradable antibacterial fiber and a preparation method thereof, and relates to the technical field of fibers. When the degradable antibacterial fiber is prepared, 2-methyl benzoic acid firstly reacts with methanol, then reacts with hydrazine hydrate, and finally reacts with S-iso-methyl thiourea methyl sulfate to prepare the antibacterial agent. The preparation method comprises the following steps: carrying out dehydration condensation on 1, 4-butanediol, 1, 5-glutaric acid, a modified flame retardant and 1, 2, 3, 4-cyclobutanetetracarboxylic dianhydride to prepare modified polyester; the preparation method comprises the following steps: reacting nano titanium dioxide with hydrolyzed 3-aminopropyltrimethoxysilane, and then reacting with thiodipropionic acid to obtain the modified nano titanium dioxide. And mixing the modified polyester with the modified nano titanium dioxide, and carrying out melt spinning to obtain the modified polyester fiber. And treating the modified polyester fiber with a post-treatment solution prepared from the antibacterial agent to obtain the degradable antibacterial fiber. The degradable antibacterial fiber prepared by the preparation method disclosed by the invention has excellent degradability and antibacterial property.

The invention relates to a cyclobutane derivative and application thereof in medicine, in particular to a compound shown in a general formula (I) or a stereoisomer, a tautomer, a racemate, pharmaceutically acceptable salt and an intermediate thereof, and application of the compound in inhibiting or degrading AR related diseases such as cancers. And B-L-K (I).

The invention discloses a high-transparency and high-impact amorphous copolyester, which relates to the technical field of high polymer materials and is prepared from dibasic acid and dihydric alcohol through esterification condensation polymerization. The dihydric alcohol comprises one or two dihydric alcohol with irregular structures; the dihydric alcohol with the irregular structure is selected from any one of 1, 4-cyclohexanedimethanol, neopentyl glycol, spiro ethylene glycol, isosorbide, and 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol; the binary acid is one or more of terephthalic acid, isophthalic acid and 2, 6-naphthalic acid. The amorphous copolyester has the advantages of high transparency, high impact resistance and high heat resistance.

A method of treating cancer cells to achieve apoptosis including contacting the cancer cells with a porous particulate nanocomposite in an amount sufficient to kill the cancer cells. The porous particulate nanocomposite contains a magnetic nickel ferrite (NiFe2O4) having an inverse spinel crystal structure; and, monodisperse spherical silica (Sil) particles onto which the magnetic NiFe2O4 is dispersed. The nanocomposite is functionalized with cis-diammine (cyclobutane-1,1-dicarboxylate-O,O′)platinum(II) (carboplatin or Carbpt) and folic acid (FA). The cancer cells are cells of colon cancer, colorectal cancer and / or cervical cancer.