135results about "Steroids preparation" patented technology

The present invention relates to a process for preparing B-[(7α,17β)-17-hydroxy-7-[9-[(4,4,5,5,5-pentafluoropentyl)sulfinyl]nonyl]estra-1,3,5(10)-trien-3-yl]-boronic acid, also known as Fulvestrant-3-boronic acid or ZB716, whose structure is reported below.

The invention discloses a method for increasing the content of diammonium glycyrrhizinate, and aims to solve the problems of low solubility, unstable crystallization and easy degradation in the existing purification process. The method comprises the following steps: adding a diammonium glycyrrhizinate crude product and hydroxypropyl-beta-cyclodextrin into purified water at normal temperature to prepare a homogeneous solution; adding stronger ammonia water to obtain ammoniated liquid; raising the temperature to 35-40 DEG C at the speed of 1-2 DEG C / min and Adding 90% ethanol and maltitol to prepare a stable crystallization solution; dropwise adding glacial acetic acid to adjust the pH value to 4-5, standing and crystallizing for 12-14 hours, filtering, leaching with purified water at 40-45 DEG C, and performing vacuum freeze drying to obtain a finished product. According to the method, the hydroxypropyl-beta-cyclodextrin is used for solubilization, the maltitol is used for stable crystallization, the process is mild and free of degradation, the purity of the finished product is high, no solvent is left, and the method is suitable for industrial production of pharmaceutical-grade diammonium glycyrrhizinate.

The invention belongs to the field of traditional Chinese medicine chemistry and natural product separation, and particularly relates to extraction and separation of a novel triterpenoid compound 25-Etherxy-dammar-20 (22) Z-ene-3beta, 6alpha, 12beta-triol and application of the novel triterpenoid compound 25-Etherxy-dammar-20 (22) Z-ene-3beta, 6alpha, 12beta-triol in myocardial protection drugs. The compound is named as 25-Etherxy-dammar-20 (22) Z-ene-3beta, 6alpha, 12beta-triol, and the structural formula of the compound is shown in the description. The invention provides an extraction and separation method of the compound. The extraction and separation method mainly comprises the following steps: sequentially carrying out solvent extraction, macroporous adsorption resin enrichment, silica gel column chromatography, ODS medium-pressure column chromatography, high performance liquid chromatography separation and purification and the like on ginseng and other traditional Chinese medicine processed products and hydrolysates. The structure of the compound is determined through comprehensive analysis of a high-resolution mass spectrum (HRMS), one-dimensional nuclear magnetic resonance (1H NMR, 13C NMR) and a two-dimensional nuclear magnetic resonance spectrum (such as HSQC, HMBC, ROESY and the like), and the compound is a newly discovered dammarane type triterpene compound. Experiments show that the compound and the composition thereof have a remarkable protection effect on myocardial cell hypoxia / reoxygenation reperfusion injury, and can be used for preparing drugs for preventing or treating myocardial ischemia reperfusion injury and other related diseases.

The invention relates to the technical field of cholesterol preparation, and discloses a preparation method of plant-derived cholesterol, which comprises the following steps: 1) heating and dissolving phytosterol with n-amyl alcohol, adding stigmasterol until saturation, cooling and crystallizing, and then carrying out solid-liquid separation to obtain a stigmasterol crude product; 2) heating and dissolving the stigmasterol crude product with absolute ethyl alcohol, adding pyridine, and continuously dropwise adding acetic anhydride for reaction; after the reaction is completed, adding deionized water for mixing, extracting with n-hexane for multiple times, separating an upper-layer oil phase, and concentrating and drying the oil phase to obtain a white solid; 3, the white solid is subjected to oxidation reduction, witting reaction and hydrogenation reaction, and cholesterol is obtained.The method has the advantages that compared with the prior art that the plant source cholesterol is directly prepared from the raw material phytosterol, the process is simplified, and meanwhile the product yield can be increased.

The present invention provides a process for Pd(II) -catalyzed site selective β- and γ-C(sp3)-H arylation of primary aldehydes controlled by transient directing groups.

The invention belongs to the technical field of biological medicines, and provides a method for synthesizing testosterone 17-O-beta-D-glucosyl-(1-> 4)-6 ''-O-acetyl-beta-D-glucoside through two-step enzymatic coupling. Mainly relates to an intermediate compound testosterone 17-O-beta-D-glucosyl-(1-> 4)-beta-D-glucoside for synthesizing the molecule, mutant amino acid and nucleotide sequences of glycosyl transferase OsSGT2 for synthesizing the intermediate, and synthesis application. In addition, the invention also provides an application of the testosterone 17-O-beta-D-glucosyl-(1-> 4)-6 ''-O-acetyl-beta-D-glucoside in liver protection.

The group of inventions relates to the field of medicine, pharmacology and the chemical and pharmaceutical industry and includes an improved method for producing (10S, 13S, 16R, 17R)-17-hydroxy-10,13,16-trimethyl-17-propanoyl-7,8,12,14,15,16-hexahydro-6H-cyclopenta[a]phenanthrene-3-one (compound of formula (I)) and the use thereof for industrial batch, semi-continuous and continuous chemical production. Also described is a method for producing an intermediate compound, Vamorolone Acetate. The method for producing the compound of formula (I) is carried out according to the schema depicted. The production method makes it possible to produce the compound of formula (I) with a purity suitable for the use thereof in a finished dosage form for subjects requiring treatment for Duchenne muscular dystrophy. Thus, the technical results of the present invention consist in an improved production method which results in: a high yield and chemical purity, including stereoisomeric purity, of the compound of formula (I) and intermediate products in the synthesis of the compound of formula (I), which are suitable for use in a finished dosage form for subjects requiring treatment for Duchenne muscular dystrophy; the adaptability of the synthesis of the compound of formula (I) to industrial production; environmentally-friendly production; and a decrease in the formation of undesirable by-products.

The invention discloses a marsdenia tenacissima extract as well as a preparation method and application thereof, and belongs to the technical field of medicines. The marsdenia tenacissima extract is Marsdenside A or Marsdenside C, and the structural formulas of the marsdenside A and the Marsdenside C are respectively shown as a formula I and a formula II. Marsdenside C can induce ferroptosis and inhibit liver cancer, and the liver cancer is liver cancer caused by HepG2 or Huh7 cells; the Marsdenside A induces pyroptosis to play a role in inhibiting the gastric cancer, and the gastric cancer is caused by HGC-27 or AGS cells, so that the Marsdenside C can be used for preparing the medicine for resisting the liver cancer, and the Marsdenside A can be used for preparing the medicine for resisting the gastric cancer.

The invention belongs to the technical field of medicines, and discloses an arbutin amino acid derivative as well as a preparation method and application thereof. According to the invention, a microbial conversion technology is utilized, the arbutin is taken as a substrate, pyroglutamic acid is introduced to the 28 site of the arbutin in a regioselective manner, and the arbutin-28beta-pyroglutamate with a novel structure is obtained. An in-vitro anti-tumor cell test proves that the compound has remarkable anti-tumor activity and can be used as an active component of an anti-tumor drug. A mouse in-vivo experiment proves that the compound has a remarkable anti-osteoporosis effect, can be used as an active ingredient of an anti-osteoporosis medicine, and has wide application.

The invention provides maslinic acid PROTACs as well as a preparation method and application thereof, and belongs to the technical field of drug development. According to the invention, maslinic acid is taken as a POI ligand, lenalidomide and fluoro-thalidomide are taken as E3 ligands, and linker selects a PEG chain or an aliphatic chain, so that the anti-cancer activity of the compound is superior to that of maslinic acid, and the compound has a good potential application prospect in the aspect of anti-tumor treatment.

The present invention relates to the technical field of pharmaceutics, and in particular to a triptolide lignocerate, a liposome thereof and a preparation method therefor. The chemical structural formula of the triptolide lignocerate is represented by formula (I). The triptolide lignocerate provided by the present invention is obtained by esterification of triptolide C14-OH and lignoceric acid. The anti-tumor effectiveness, safety and the like of the triptolide lignocerate liposome are further improved with respect to the prior art, so that a foundation is laid for providing safer and more effective triptolide-related clinical preparations.

The invention provides a method for catalytically synthesizing 7-amino-3-oxabicyclo [3.3. 1] nonyl-6-ene-1-ol by using rare earth, which comprises the following steps of: adding a catalyst and a catalyst, according to the preparation method, rare earth trifluoromethanesulfonate is taken as a catalyst, 6-alkoxy-2, 6-dihydropyran-3-ketone and enamine compounds are taken as raw materials, and the 7-amino-3-oxabicyclo [3.3. 1] nonyl-6-ene-1-ol is prepared by catalyzing (3 + 3) cyclization reaction. The synthesis method provided by the invention is simple in reaction raw material synthesis, low in rare earth salt price, easy in experimental operation and suitable for large-scale preparation. The obtained compound can be applied to the fields of organic synthesis, drug synthesis, organic materials and the like.

The invention relates to a synthetic method of didrogesterone. According to the method, progesterone is subjected to ketalation, halogenation, elimination, illumination isomerization, deprotection and final isomerization, and the didrogesterone is obtained. The method has the advantages of high yield, cheap and easily available raw materials, green and safe whole process route, high bulk drug quality and purity of 99.8% or more, and is suitable for industrial production.

The present invention provides a process for Pd(II)-catalyzed site selective β- and γC(sp3)-II arylation of primary aldehydes controlled by transient directing groups.

The application relates to the technical field of organic synthesis, and particularly discloses a synthesis process of high-purity pregnenolone, which comprises the following steps: S1, esterification reaction of progesterone and an acylation reagent to obtain product 1; S2, ketalization reaction of the product 1, diol and a dehydrating agent in the presence of a catalyst to obtain product 2; S3, reduction reaction of the product 2 and a reducing agent to obtain product 3; and hydrolysis reaction of the product 3 and an acidic compound to obtain pregnenolone. The synthesized pregnenolone has high purity and yield.

The invention discloses a synthesis method of 8, 9-dehydroestrone. The invention discloses a preparation method of 8, 9-dehydroestrone, which comprises the following steps: (1) in the presence of an acid catalyst, in an aprotic solvent, carrying out a deprotecting group-isomerization reaction on a compound 5 to obtain a compound 6; and (2) in the presence of a catalyst, in an aprotic solvent, carrying out an addition reaction on the compound 6 and a hydrogen source reagent to obtain the 8, 9-dehydroestrone. The method has one or more advantages as follows: raw materials are cheap, reaction steps are simple, the reaction yield of each step is high, post-treatment is simple and convenient, conditions are mild, operation is controllable, and the method is suitable for amplification.

The invention provides a method for catalytically synthesizing 7-oxa-2-azabicyclo [3.3. 1] nonyl-3-ene-1-ol by using rare earth, which comprises the following steps of: adding a catalyst and a catalyst, according to the preparation method of the 7-oxa-2-azabicyclo [3.3. 1] nonyl-3-ene-1-ol, rare earth trifluoromethanesulfonate is taken as a catalyst, 6-alkoxy-2, 6-dihydropyran-3-ketone and enamine compounds are taken as raw materials, and the preparation of the 7-oxa-2-azabicyclo [3.3. 1] nonyl-3-ene-1-ol is realized. The method is simple in reaction raw material synthesis, simple in experimental operation and suitable for large-scale preparation. The obtained compound can be applied to the fields of organic synthesis, drug synthesis and the like.

The invention discloses a pentacyclic triterpene acylhydrazone compound as well as a preparation method and application thereof. A series of oleanolic acid derivatives are synthesized by carrying out structural modification on carboxyl at C28 site of oleanolic acid, structural confirmation is carried out by using 1H NMR, 13C NMR, HRMS and X-ray single crystal diffraction, and the inhibition effect of the pentacyclic triterpenoid acylhydrazone compound on the activity of tumor cells A549, AGS and K562 is evaluated by taking cis-platinum as positive control and adopting a CCK-8 method. Results show that the inhibition effect of the derivatives 5, 6, 9, 10, 16, 21, 27 and 28 on tumor cells is superior to that of cis-platinum. Reference is provided for research of oleanolic acid derivatives and discovery of anti-tumor seedling compounds.

The invention relates to the technical field of pharmaceutical chemicals, in particular to a refining method of an eplerenone intermediate. The method comprises the following steps: S1, dissolving: sequentially adding an eplerenone methyl ester crude product, an organic solvent and water into a reaction bottle, and stirring and heating to completely dissolve the eplerenone methyl ester crude product, the organic solvent and the water; s2, reaction: adding inorganic alkali into a dissolved reaction system, and stirring for full reaction at controlled temperature; s3, elutriation: cooling the system to room temperature, and slowly dropwise adding water to precipitate a solid product; s4, devitrification: cooling, devitrifying and fully stirring; s5, filtering and drying: filtering the system for solid-liquid separation, and drying to obtain an eplerenone methyl ester fine product. The eplerenone methyl ester refining method provided by the invention is high in product yield and low in cost, the adopted organic solvent is a common solvent and is low in toxicity, and the eplerenone methyl ester refining method has good industrial application value and is very suitable for large-scale industrial application.

The invention discloses an extraction method of 5 alpha-carp cholesteryl sulfate, and belongs to the technical field of extraction and purification of bile acid active substances. The extraction method of 5 alpha-carp cholesteryl sulfate comprises the following steps: (1) carrying out freeze drying or rotary evaporation concentration on fresh fish bile to obtain a crude product; (2) mixing and dissolving the crude product obtained in the step (1) with hot methanol at 50-80 DEG C according to a mass ratio of the crude product to the methanol of 1: (5-10), carrying out suction filtration while the crude product is hot, and collecting filtrate; and (3) ethyl acetate is added into the filtrate obtained in the step (2), the mass ratio of the methyl alcohol to the ethyl acetate is 1: (1-2), standing is conducted, a solid is separated out, and the obtained solid is the 5 alpha-carp cholesteryl sulfate. The extraction method disclosed by the invention is simple and convenient, high in yield, high in product quality and low in cost.

The present invention relates to a compound for the prevention and / or treatment of neurodegenerative diseases. On one hand, the compound provided by the invention can effectively promote the proliferation of neuronal cells, and on the other hand, the compound has a protection effect on neuronal cell toxicity induced by neurotransmitters such as glutamic acid caused by excessive accumulation of Abeta amyloid protein, so that the effect of treating neurodegenerative diseases is comprehensively exerted; meanwhile, the compound disclosed by the invention has no obvious cytotoxicity. Therefore, the compound has a good application prospect in medicines for preventing or treating neurodegenerative diseases such as Alzheimer's disease, Parkinson's disease, Huntington's disease and the like. Besides, a parent structure with a key active function on the neurodegenerative disease and an important influencing group in the cynanchum otophyllum extract are defined, the basic structure-function relationship between the compound and the treatment of the neurodegenerative disease is defined, and a sufficient scientific basis is provided for research and development of subsequent related drugs.

Steroid acid-based hydrogels and methods of production thereof are described herein. More specifically, the present description relates to steroid acid-peptide conjugates for the formation of a hydrogel. Peptides are covalently conjugated to a one or more of steroid acid moieties and dissolved or resuspended in a solvent to form a hydrogel. The steroid acids may include bile acids and bile acid analogs. The peptides may include a nuclear localisation signal (NLS).

Steroid acid-peptide conjugates covalently modified for improved stability and / or biological activity are described herein. Covalent modifications include the formation of multimeric compounds comprising at least two steroid acid-peptide monomers covalently bound to one another that behave as new chemical entities, as well as protecting one or more free thiol groups present in the steroid acid- peptide conjugates to improve their stability and / or biological activity.

The invention relates to the technical field of separation and purification of active ingredients of traditional Chinese medicines, and discloses a saponin compound derived from aralia elata and a preparation method thereof. The saponin compound has a structure as shown in a formula (I). The preparation method comprises the following steps: carrying out hydrous ethanol extraction on aralia mandshurica root bark, enriching through macroporous adsorption resin, carrying out directional enrichment on acidic saponin through anion exchange resin, carrying out coarse separation and preparative liquid phase refining by adopting reversed-phase C18 chromatography, and carrying out window collection in combination with online detection to obtain a target saponin compound. The method can improve the separation selectivity of the target component, reduce the co-elution phenomenon and improve the purity and batch stability of the final product, and is suitable for preparation of the aralia mandshurica sourced saponin compound.

The invention discloses a preparation method of a steroid compound. Specifically, the invention discloses a preparation method of (3S, 10R, 13S)-10, 13-dimethyl-17-(4-methyl-1H-imidazole-1-yl)-2, 3, 4, 7, 8, 9, 10, 11, 12, 13, 14, 15-dodecahydro-1H-cyclopentadiene [a] phenanthrene-3-ol, and a preparation method of the (3S, 10R, 13S)-10, 13-dimethyl-17-(4-methyl-1H-imidazole-1-yl)-2, 3, 4, 7, 8, 9, 10, 11, 12, 13, 14, 15-dodecahydro-1H-cyclopentadiene [a] Compared with the prior art, the method disclosed by the invention has the advantages of few reaction steps, simplicity in operation, low cost, high yield, greenness, environmental friendliness and the like, and the final product does not need column chromatography purification, is more suitable for large-scale production and is beneficial to popularization.

The present invention discloses a method for synthesizing high-purity plant-derived cholesterol, which uses plant-derived 21-hydroxy-20-methylpregn-4-en-3-one, also known as bisnoral alcohol or BA, as raw material, and can synthesize the above cholesterol through steps such as oxidation, Wittig reaction, acetylation, reduction, selective hydrogenation reduction, or can synthesize the above cholesterol through steps such as oxidation, Wittig reaction, acetylation, reduction, hydroxyl protection, selective hydrogenation reduction, deprotection or hydrolysis, and the purity can reach 99% or more. Considering the shortcomings of traditional animal-derived cholesterol, the present invention synthesizes cholesterol from plant-derived raw material BA, which is not only safe and avoids the risk of pathogenic bacteria and virus infection, but also has a high synthesis yield, good product purity, environmentally friendly, and convenient for industrialized production, and the present invention greatly reduces the level of impurities in the product, making it easy to obtain high-purity cholesterol and improving the safety of clinical use.

The invention relates to the technical field of medicines, in particular to a preparation method of high-purity single crystal form betamethasone acetate, which comprises the following step: sequentially contacting a betamethasone acetate crude product with acetone and methanol to obtain an I alpha crystal form betamethasone acetate crystal. According to the method, acetone and methanol are adopted as crystallization solvents, isomeride impurities which are difficult to remove can be effectively removed, a single crystal form sample with few impurities and high purity is obtained, and the purification problem that the impurities are difficult to remove and the problem that crystals are easy to mix when betamethasone acetate is used as a polycrystalline compound are solved. The obtained I alpha crystal form is a single crystal form, is good in physical and chemical stability, regular in crystal form, good in granularity uniformity and good in fluidity, overcomes the defects that in the prior art, the crystallization process is tedious, materials are high in electrostatic property and prone to floating and adhering to walls, and particles are not uniform, and has excellent properties in the aspect of processing adaptability. The method is simple, efficient, convenient to operate, high in repeatability, small in pollution and good in impurity removal effect, meets the factory GMP production requirement and is suitable for industrial production.