29 results about "Butylone" patented technology

The application relates to the technical field of chemical synthesis, in particular to a synthesis method of a key intermediate of pentconazole, which comprises the following steps: S1, Witting-Horner reaction of 2,4-dichlorobenzophenone and (diethoxy) phosphoethyl acetate under the action of a strong base to generate 3-(2,4-dichlorophenyl)-2-en-hexanoic acid ethyl ester; S2, Prilezhaev epoxidation reaction of 3-(2,4-dichlorophenyl)-2-en-hexanoic acid ethyl ester and meta-chloro peroxybenzoic acid to generate 3-(2,4-dichlorophenyl)-2,3-epoxy-hexanoic acid ethyl ester; and S3, base hydrolysis and acidification of 3-(2,4-dichlorophenyl)-2,3-epoxy-hexanoic acid ethyl ester to obtain a key intermediate 2-(2,4-dichlorophenyl) pentanal of pentconazole. The application has the effects of higher reaction yield, lower toxicity of reaction raw materials and more gentle reaction conditions.

The invention discloses a method and a system for preparing a 4-AA medical intermediate through continuous flow ozone oxidation. The method comprises the following steps: continuously introducing a raw material solution containing (3R)-3-((R)-1-((tert-butyldimethylsilyl) oxy) ethyl)-1-(4-methoxyphenyl)-4-oxo azetidine-2-yl acetate and a gas containing ozone into a microreactor for reaction; after the reaction liquid is subjected to reduction quenching, the (3R, 4R) 4-acetoxyl-3-[R-(tert-butyldimethylsiloxy) ethyl]-2-azetidinone is obtained. On one hand, the reaction time is shortened from the hour level to the minute level, and the production efficiency is remarkably improved; and on the other hand, the reaction temperature is increased to 10-30 DEG C from deep cooling, so that the refrigeration energy consumption and the equipment requirement are greatly reduced. According to the invention, local peroxidation is fundamentally avoided, byproducts are obviously reduced, the product purity is improved, the method is suitable for continuous operation, the reaction process is controllable, and the method is safe and reliable.

The application provides a transaminase, the amino acid sequence of which is shown as SEQ ID NO. 3, which can catalyze the conversion of (2Z)-4-oxo-4-[3-(trifluoromethyl)-5,6-dihydro[1,2,4]triazolo[4,3-a]pyrazin-7-(8H)-yl]-1-(2,4,5-trifluorophenyl)butan-2-one into sitagliptin in a methanol solution reaction system.

The invention discloses an ultrahigh-temperature ceramic film with improved conductivity through grafting modification and a preparation method of the ultrahigh-temperature ceramic film, and relates to the technical field of ultrahigh-temperature ceramic preparation. The method comprises the following steps: stirring and dispersing a SiHfBCN ceramic precursor polymer, MWCNTs-COOH and triton X-100 in methylbenzene, then adding 2-benzyl-2-dimethylamino-4 '-morpholinyl phenylbutanone, and stirring and dissolving to prepare a mixed solution; spin-coating on the surface of a pretreated silicon wafer to prepare a polymer film; and carrying out ultraviolet irradiation, pyrolyzing and cooling to prepare the ultrahigh-temperature ceramic film with improved conductivity through grafting modification. The room temperature resistivity of the modified SiHfBCN ceramic thin film can be reduced by about 70% to the maximum, and the problem that an existing ceramic thin film is poor in conductivity is solved.

The invention relates to an antimicrobial mixture containing 4-(3-ethoxy-4-hydroxyphenyl)butan-2-one and an additional compound chosen from a monovalent or divalent metal salt of pyrithione, piroctone olamine, diazolidinylurea, a hexamidine compound, and imidazolidinylurea,and also to a cosmetic composition containing such a mixture.Application to caring for, making up and cleansing keratin materials.

This invention relates to a method for synthesizing squaric acid, the method comprising the following steps: (1) reacting alkyl vinyl ether, trichloroacetyl chloride, and zinc to obtain 2,2-dichloro-3-alkoxycyclobutanone; (2) subjecting 2,2-dichloro-3-alkoxycyclobutanone to chlorination with chlorine to obtain 2,2,4,4-tetrachloro-3-alkoxycyclobutanone; (3) subjecting 2,2,4,4-tetrachloro-3-alkoxycyclobutanone to elimination reaction with a base to obtain 2,4,4-trichloro-3-alkoxycyclobuten-1-one; and (4) subjecting 2,4,4-trichloro-3-alkoxycyclobuten-1-one to hydrolysis to obtain the squaric acid. The synthesis method provided by this invention avoids the use of the prohibited raw material perchloro-1,3-butadiene and has lower energy consumption, meeting the needs of green and clean production.

The invention discloses a peptide simulant and a preparation method thereof, 3-oxetanone and 3-methyl-1-nitrobutane are used as raw materials, and all reactions are carried out to obtain a target product. The peptide simulant is novel in structure and has potential biological activity, adopted protecting groups and functional groups are good in compatibility, and follow-up structural modification is facilitated; the designed synthesis route is simple, the reaction condition is mild, and amplification is easy; the yield of each step is high, and the product is easy to purify.

This invention discloses a benzamide / benzenesulfonamide compound containing an aryl butanone structure, its preparation method, and its application, belonging to the field of medicinal chemistry. The structure of the benzamide compound containing the aryl butanone structure is as follows: R1 is hydrogen, halogen, alkyl, or alkoxy; R2 is tert-butyl, tert-pentyl, tert-octyl, adamantyl, or α,α-dimethylbenzyl; R3 is hydrogen, halogen, alkyl, alkoxy, fused ring, or aryl; R4 is hydrogen, alkyl, or aryl. The structure of the benzenesulfonamide compound containing the aryl butanone structure is as follows: R1 is hydrogen, halogen, or alkyl; R2 is tert-butyl, tert-pentyl, or tert-octyl; R3 is hydrogen, halogen, alkyl, or fused ring. The advantages of this invention are that some of the prepared compounds exhibit strong inhibitory effects on MCF-7 and HCT-116, and can be used as lead compounds for the subsequent preparation and development of antitumor drugs.

The present disclosure is directed, in general, to synthesizing optionally substituted 2-dicyanomethylene-3-cyano-4-methyl-5-phenyl-5-perfluoromethyl-2,5-dihydrofuran comprising (i) reacting tributyl (1-ethoxyvinyl) tin with n-butyllithium at a temperature of between −30° C. and 10° C. to produce a first reaction product; (ii) reacting the first reaction product with 2,2,2-trifuoroacetophenone to produce a second reaction product: (iii) quenching the second reaction product with an acid to produce 3-hydroxy-3-phenyl-4,4,4-trifluoro-2-butanone; and (iv) reacting the 3-hydroxy-3-phenyl-4,4,4-trifluoro-2-butanone with malononitrile in the presence of base to produce 2-dicyanomethylene-3-cyano-4-methyl-5-phenyl-5-perfluoromethyl-2,5-dihydrofuran.

This invention discloses a method for synthesizing a key intermediate compound of rumepiride and its preparation, belonging to the field of pharmaceutical intermediates technology. This invention discloses for the first time a novel rumepiride-specific key intermediate, 1-(4-fluorophenyl)-4-(4-piperidinone-1-yl)but-1-one, whose structure is precisely adapted to the requirements of constructing the tetracyclic core of rumepiride, exhibiting excellent chemical stability and reactivity. This invention provides two independent preparation processes for γ-hydroxybutyric acid and γ-aminobutyric acid, adaptable to different raw material supply scenarios. The high-purity intermediate is prepared through halogenation, Friedel-Crafts acylation, nucleophilic condensation or double addition, Dickmann condensation, and hydrolysis decarboxylation steps. The process of this invention is simple to operate, has mild conditions, few side reactions, and stable yield. The purity of the prepared intermediate is ≥99.5%, and the impurity index meets the application standards for high-end active pharmaceutical ingredients. It can directly undergo a cyclization reaction with 2-(methylamino)phenylhydrazine to construct the rumepiride nucleus, effectively solving the pain points of existing technologies such as cumbersome processes, low yield, and difficulty in controlling impurities. It fills a technological gap in the industry and has extremely high industrial production value and patent application prospects.

The invention relates to a method for synthesizing squaric acid, which comprises the following steps of: (1) reacting alkyl vinyl ether, trichloroacetyl chloride and zinc to obtain 2, 2-dichloro-3-alkoxy cyclobutanone; (2) carrying out a chlorination reaction on the 2, 2-dichloro-3-alkoxy cyclobutanone and chlorine gas to obtain 2, 2, 4, 4-tetrachloro-3-alkoxy cyclobutanone, and carrying out a chlorination reaction on the 2, 2-dichloro-3-alkoxy cyclobutanone and chlorine gas to obtain 2, 2, 4, 4-tetrachloro-3-alkoxy cyclobutanone; (3) the 2, 2, 4, 4-tetrachloro-3-alkoxy cyclobutanone and alkali are subjected to an elimination reaction, and 2, 4, 4-trichloro-3-alkoxy cyclobutene-1-one is obtained; and (4) carrying out a hydrolysis reaction on the 2, 4, 4-trichloro-3-alkoxy cyclobutene-1-ketone, so as to obtain the squaric acid. The synthesis method provided by the invention can avoid the use of a forbidden raw material perchloro-1, 3 butadiene, also has lower energy consumption, and can meet the requirements of green and clean production.

The application belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of apalutamide. The preparation method comprises the following steps: 4-amino-2-fluoro-N-methyl benzamide is reacted with 1-bromocyclobutane-1-methyl carboxylate under the catalysis of silver oxide, the obtained product is reacted with 5-isothiocyanate-3-(trifluoromethyl) pyridine-2-cyan to obtain apalutamide; the starting material is cheap and easy to obtain, and the existing technology avoids the Strecker reaction of N-methyl-2-fluoro-4-amino benzamide, sodium cyanide (or trimethyl silyl cyanide) and cyclobutanone, which needs to use a toxic cyanide reagent; meanwhile, the Ullmann reaction needs high temperature and equivalent copper, and the application solves the problems, and is simple to operate, has a higher yield, and is more suitable for industrial mass production.

The present invention relates to a method for producing enantiomerically enriched cyclobutylamine of formula (I) from alpha-tert-cyclobutanone and reacting said enantiomerically enriched cyclobutylamine to obtain enantiomerically enriched cyclobutyramide. Such compounds are useful intermediates in the synthesis of microbicidal thiazole compounds. (I)

The invention relates to the technical field of drug synthesis equipment, in particular to an olmesartan medoxomil phosgene substitution type acylation reaction system, which comprises a reaction container, a reaction kettle, a reaction kettle and a control system, the triphosgene adding device is connected with the reaction container and is used for quantitatively adding triphosgene into the reaction container; the solvent conveying unit is connected with the reaction container and is used for pumping a solvent into the reaction container; the mixed solution feeding unit is connected with the reaction container and is used for slowly adding a mixed solution of 3-hydroxybutanone and a solvent into the reaction container; the temperature control module is connected with the reaction container and is used for accurately controlling the reaction temperature in the reaction container; and the pH adjusting and quenching unit is connected with the reaction container. According to the invention, the triphosgene adding device and the closed system are adopted to completely replace highly toxic gas phosgene, so that major potential safety hazards in the production, storage and transportation processes are fundamentally solved.

The application provides a high-transparency low-shrinkage TPU film and a preparation method thereof. The preparation raw material of the high-transparency low-shrinkage TPU film comprises the following components in parts by weight: 100 parts by weight of TPU particles, 30-60 parts by weight of polycarbonate, 0.1-0.5 parts by weight of (4-hydroxycyclohexyl)methyl) tert-butyl carbamate, 0.5-1 parts by weight of 1-(2,4-dihydroxy-3-trifluoromethyl-phenyl)-3-methyl-butan-1-one and 1-3 parts by weight of an antioxidant. The shrinkage of the TPU film is as low as 0.1% or below, the TPU film has good transparency, the light transmittance is 98.5% or above, the mechanical strength is high, and the TPU film is suitable for multiple fields such as automobiles, household appliances, electrical instruments, mechanical industry and the like.

The application provides a special sealant for simulation cake shaping and a preparation method thereof, and relates to the technical field of adhesives.The raw material composition of the sealant comprises alpha, omega-dihydroxypolydimethylsiloxane, methyltributanone oxime silyl, a catalyst, a composite regulator, edible-grade white oil, gamma-aminopropyltriethoxysilane, nano calcium carbonate loaded blocked isocyanate and deionized water.The catalyst is dibutyltin dilaurate; and the composite regulator is a mixture of modified nano silicon dioxide and an antioxidant.The special sealant for simulation cake shaping prepared by the application has the advantages of short setting time, excellent aging resistance and environmental protection.

This disclosure provides novel transmucosal and subcutaneous pharmaceutical compositions and methods of preparation and use thereof, the pharmaceutical compositions comprising 1-(4-fluoro-phenyl)-4-((6bR,10aS)-3-methyl-2,3,6b,9,10,10a-hexahydro-1H,7H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxalo-8-yl)-but-1-one or 1-(4-fluoro-phenyl)-4-((6bR,10aS)-2,2-d2-3-methyl-2,3,6b,9,10,10a-hexahydro-1H,7H-pyrido[3′,4′:4,5]pyrrolo[1,2,3-de]quinoxalo-8-yl)-but-1-one in the form of a free base, eutectic or salt.

The application discloses a kind of methyl acrylate-acetonitrile-water ternary azeotrope extractant and extraction separation method, and the extractant is one of methyl isobutyl ketone, butyl acetate;Extraction separation method includes intermittent extraction separation or continuous extraction separation method, intermittent extraction separation method is mixed with methyl acrylate-acetonitrile-water ternary azeotrope and extractant, according to the selective difference of extractant to methyl acrylate and acetonitrile Determine the production sequence, collect tower top fraction by controlling reflux ratio, operating pressure and temperature respectively;Continuous extraction separation method is by extraction rectification column, extraction recovery column and extractant dehydration tower to methyl acrylate-acetonitrile-water ternary azeotrope carries out continuous extraction separation of methyl acrylate, acetonitrile, water.The extractant of the application has good extraction separation effect on methyl acrylate-acetonitrile-water ternary azeotrope, so that the purity of methyl acrylate reaches more than 99%, the yield reaches more than 97%, the purity of acetonitrile reaches more than 98.5%, and the yield reaches more than 96.5%.

The invention relates to a Papililone A tetracyclic diterpenoid analogue and a preparation method and application thereof, the Papililone A tetracyclic diterpenoid analogue has the following structural formula: R1, R2, R3, R4 and R5 are selected from hydrogen, alkyl and aryl, the Papililone A tetracyclic diterpenoid analogue is synthesized by carrying out diastereoselective 2 + 2 reaction on a cyanoalkene substrate to construct a cyclobutanone fragment, the other fragment is a constructed furan bromide, and the structural formula is shown in the specification. Performing bromine lithium exchange on furan bromide fragments, performing nucleophilic addition on the furan bromide fragments and cyclobutanone to connect the fragments, and performing photooxidation ring opening to construct an alkene-inserted alpha-hydroxy ketone rearrangement substrate. Under the alkaline condition, rearrangement is carried out, and the diquinane with two continuous quaternary carbon chiral centers is successfully constructed. The preparation method comprises the following steps: firstly, synthesizing tetracyclic diterpenoid, then selectively converting a substrate into trifluoromethanesulfonic acid alkenyl ester, and then carrying out carbonyl alpha-position alkenylation reaction and alkenyl insertion Michael reaction under the action of metal, so as to efficiently and concisely synthesize the tetracyclic diterpenoid natural product Papililone A for the first time. A series of Papililone A tetracyclic diterpenoid analogues are rapidly synthesized by adopting the synthesis method disclosed by the invention.

The invention belongs to the technical field of coatings, and discloses a multi-component anti-skinning composition based on oxime and an application of the multi-component anti-skinning composition. The compound is composed of oxime compounds, and specifically comprises acetoxime, propionaldehyde oxime, 2-butanone oxime, butyraldehyde oxime, 2-pentanone oxime, 3-pentanone oxime, methyl isopropyl ketoxime, methyl isobutyl ketoxime, pinacol oxime, cyclopentanone oxime, 2-hexanone oxime, 3-hexanone oxime, cyclohexanone oxime, 2, 2, 4, 6-tetramethyl-3-pentanone oxime, 2, 2, 4, 6-tetramethyl-3-pentanone oxime, 2, 2, 4, 6-tetramethyl-3-pentanone oxime, 2, 2, 4, 6-tetramethyl-3- the compound is selected from three or more of 3, 4, 4-tetramethyl-3-pentanone oxime, 4-methyl-2-pentanone oxime, 2-heptanone oxime, 3-heptanone oxime, 4-heptanone oxime, cycloheptanone oxime, 2-nonanone oxime, 5-methyl-2-hexanone oxime, 5-methyl-3-heptanone oxime, 6-methyl-2-heptanone oxime, benzaldoxime and acetophenone oxime. The anti-skinning coating has more excellent anti-skinning performance, and the quality of the oxidation drying type coating can still be stable after long-time storage.

This invention belongs to the field of pharmaceutical chemistry, specifically relating to a method for preparing substituted heterocyclic fused carboline compounds. In this method, the compound of formula 3a, 4-iodo-4'-fluorophenylbutanone, and a base are reacted at low temperature, resulting in a high yield and purity of the lumepirobenone base. The method of this invention can effectively improve the quality of the finished product and is more suitable for industrial production.

The present application relates to a kind of high-efficiency synthesis method of acetone oxime and 2-pentanone oxime, belong to ketoxime synthesis technical field.The present application is added to reactor ketone or 2-pentanone, ammonia, catalyst, stir and heat, slowly drop hydrogen peroxide, reaction is carried out under closed system;After reaction, filtration, distillation under reduced pressure, obtain acetone oxime or 2-pentanone oxime;The catalyst of the present application is boron modified TS-1 molecular sieve, by TS-1 molecular sieve, vinyl tributyl ketoxime silane, methacrylic acid ester strontium, 1,2,3,4,5,6,7,8,9,10,11-undecahydro-12-mercaptododecanesulfonic acid borane, toluene, triethylamine, response is obtained;Acetone oxime and 2-pentanone oxime prepared by the present application have higher purity and yield.

The invention provides a transaminase mutant and application of the transaminase mutant in preparation of R-3-aminobutanol, and relates to the technical field of biology. The transaminase mutant provided by the invention is obtained by mutating wild type transaminase with an amino acid sequence as shown in SEQ ID NO.1, and the mutations comprise that histidine at the 62nd site is mutated into arginine, serine, threonine or cysteine, and / or glycine at the 136th site is mutated into phenylalanine. Compared with wild transaminase, the transaminase mutant has higher enzymatic activity, can efficiently catalyze 4-hydroxy-2-butanone to generate R-3-aminobutanol, and is further used for preparing dolutegravir.

The present invention relates to a new co-crystal of Gabapentin, Ketoprofen and Lysine, to pharmaceutical compositions and to their use in the prevention, reduction or treatment of pain and / or inflammation.

The invention discloses a benzamide / benzenesulfonamide compound containing an aryl butanone structure as well as a preparation method and application of the benzamide / benzenesulfonamide compound, and belongs to the technical field of medicinal chemistry. The structure of the benzamide compound containing the aryl butanone structure is as follows: R1 is hydrogen, halogen, alkyl or alkoxy; r2 is a tert-butyl group, a tert-amyl group, a tert-octyl group, an adamantyl group or an alpha, alpha-dimethyl benzyl group; r3 is hydrogen, halogen, alkyl, alkoxy, fused ring or aryl; r4 is hydrogen, alkyl or aryl. The structure of the benzenesulfonamide compound containing the aryl butanone structure is as follows: R1 is hydrogen, halogen or alkyl; r2 is tert-butyl, tert-amyl or tert-octyl; and R3 is hydrogen, halogen, alkyl or fused ring. The invention has the following beneficial effects: part of the prepared compounds have strong inhibition effect on MCF-7 and HCT-116, and can be used as drug lead compounds for subsequent preparation and research and development of antitumor drugs.

Disclosed, inter alia, are processes of preparing a compound of formula II (II), comprising reducing a compound of formula I (I), in the presence of a ketoreductase to form the compound of formula II. Also disclosed are processes of preparing a compound of formula D1, which is useful for preparing pharmaceutically active compounds such as androgen receptor (AR) degraders.

The invention discloses application of 1-hydroxy-2-butanone in preparation of a medicine for treating acute liver injury, belongs to the technical field of medicines, and particularly relates to application of 1-hydroxy-2-butanone in treatment of acetaminophen-induced liver injury. Experiments prove that 1-hydroxy-2-butanone can remarkably improve the survival rate of mice suffering from liver injury induced by acetaminophen (APAP) and remarkably relieve liver tissue necrosis and neutrophil infiltration, and serum biochemical detection further proves that when 1-hydroxy-2-butanone is adopted for treatment, the liver injury can be obviously relieved by reversing the oxidative stress level caused by APAP, and the survival rate of the mice suffering from liver injury induced by APAP can be obviously reduced. The liver function impairment caused by APAP is obviously reduced.

The present disclosure is directed, in general, to synthesizing optionally substituted 2-dicyanomethylene-3-cyano-4-methyl-5-phenyl-5-perfluoromethyl-2,5-dihydrofuran comprising (i) reacting tributyl(1-ethoxyvinyl)tin with n-butyllithium at a temperature of between -30 °C and 10 °C to produce a first reaction product; (ii) reacting the first reaction product with 2,2,2-trifuoroacetophenone to produce a second reaction product: (iii) quenching the second reaction product with an acid to produce 3-hydroxy-3-phenyl-4,4,4-trifluoro-2-butanone; and (iv) reacting the 3-hydroxy-3-phenyl-4,4,4-trifluoro-2-butanone with malononitrile in the presence of base to produce 2-dicyanomethylene-3-cyano-4-methyl-5-phenyl-5-perfluoromethyl-2,5-dihydrofuran.