48 results about "Dienedione" patented technology

The invention discloses a method of acquiring high-purity 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione, comprising the following steps: a) putting the acquired crude 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione in a proper solvent system to generate a pure 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione solid; b) separating the 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione solid; and c) carrying out recrystallization on the acquired solid. The compound used as a new oral emergency contraception can be taken in 120 h after unprotected sexual intercourse of women without a reduction of emergency contraception effect with the delay of the time of using drugs, and has good safety and survivability simultaneously.

The invention relates to a steroid compound, and a preparation method and application of the compound. The traditional method for preparing 17alpha-acetoxyl-11beta-(4-N,N-dimethylaminophenyl)19- norpregna -4,9-diene-3,20-diketone has the problems of low yield, incapability of industrial production and the like. The invention provides a novel steroid compound, and the preparation method and the application thereof. The steroid compound can be used for preparing 17alpha-acetoxyl-11beta-[4-(N,N-dimethylamino)-phenyl]-19- norpregna -4,9-diene-3,20-diketone. The preparation method is high in yield, mild in reaction condition, simple and easy to obtain raw materials and easy for industrial production.

The invention discloses a preparation method of a dydrogesterone intermediate. The preparation method is characterized by comprising the following steps: dissolving 5,7-diene steroid compound in an organic solvent to obtain a solution as a raw material; and carrying out a photocatalytic reaction and separating to obtain the dydrogesterone intermediate, wherein the 5,7-diene steroid compound is 7-dehydropregnenolone acetate, pregna-5,7-diene-3,20-diketodivinyl ketal, 7-dehydropregnenolone, ergosterol or pregna-5,7-diene-3,20-diketo-3-vinyl ketal, and a lamp used in the photocatalytic reaction comprises an LED ultraviolet lamp with the wavelength range of 295-335 nm. The preparation method of the dydrogesterone intermediate is high in yield, low in cost, safer in preparation and friendlier to environment.

The invention discloses a preparation method of a steroid intermediate. The preparation method comprises the following steps: adding a first solvent, a first acid solution, water and 17-alpha-hydroxypregnenolone steroid-4,9-diene-3,20-diketone acetate into a first reaction tank, and uniformly stirring; adding a bromination agent in four times at 2-4 DEG C, maintaining the temperature for reactingfor 2h, and carrying out thin-layer chromatography analysis until the reaction of the raw materials is finished; and regulating the pH value to be more than 7, regulating the pH value back to 6, carrying out reduced pressure concentration until the first solvent is completely concentrated, adding water, cooling to 5 DEG C, and carrying out centrifugation, cleaning, spin-drying and drying, so as toobtain the steroid intermediate, namely cortisone. According to the preparation method, an oxidant and a catalyst which contain heavy metal ions are not used, the used solvent can be recycled and reused, wastewater does not contain heavy metal ions in the production process, the method belongs to an environment-friendly process and has very good process prospects, and the yield and purity of theproduct are high.

The invention discloses 1-(4)-Hydroxy-3-Methoxyphenyl)-7- Oxyacetylcarbamoyl-AA-OBzl-Methoxyphenyl)-1,6-Heptadiene-3,5-diketone of the following formula: (wherein AA is selected from L-Lys residue, L-Asn residue, L-Pro residue, L-Gln residue, L-Ser residue and L-Thr residue), the preparation methods are disclosed, and the antitumor growth activities are disclosed, the anti-inflammatory activitiesare disclosed, thus the use in the preparation of anti-tumor drugs and anti-inflammatory drugs is disclosed. The formulas are shown in the description.

The invention relates to the field of preparation of steroid drugs and an intermediate of the same, and in particular relates to a preparation method for prednisone acetate. The method comprises the steps of taking 11 alpha, 17 alpha-dyhydroxy Pregnene-1,4-diene-3,20-dione as an initial material, oxidizing to obtain 17 alpha-hydroxy Pregnene-1,4-diene-3,11,20-trione, and carrying out iodization reacting to obtain the prednisone acetate. The invention provides a novel oxidation technology more suitable for production of the intermediate of the prednisone acetate, the synthesis path has the characteristics of low cost and simple operation, environment pollution pressure can be greatly reduce, and the yield and quality of the prednisone acetate can reach a satisfactory level.

The invention relates to a method for manufacturing a cyproterone acetate intermediate 17a-hydroxy progesterone-1, 4, 6-triene-3, 20-diketone. The method includes performing microbial fermentation and dehydrogenation on 17a-hydroxy progesterone-4, 6-diene-3, 20-diketone to obtain the 17a-hydroxy progesterone-1, 4, 6-triene-3, 20-diketone. Microbial fermentation and dehydrogenation culture media comprise 1.2-1.6(wt)% of glucose, 1.8-2.6(wt)% of corn steep liquor, 0.4-0.6(wt)% of peptone, 0.4-0.7(wt)% of potassium dihydrogen phosphate, 0.01(wt)% of defoamers and the balance water, and the pH (potential of hydrogen) of a mixture of the glucose, the corn steep liquor, the peptone and the potassium dihydrogen phosphate is regulated by a proper amount of sodium hydroxide and then ranges from 6.0 to 6.5. The method has the advantages that the microbial fermentation and dehydrogenation reaction selectivity is high, a product is free of side effects, the purity of the product is 97%, the content of the maximum impurity component is 1.5%, the yield of the product is greatly increased and reaches 80%, and environmental pollution is obviously reduced as compared with the traditional chemical synthesis process.

The invention discloses a preparation method of high-purity hydrocortisone, and belongs to the technical field of preparation and processing of medicines. According to the method, 17alpha-hydroxypregna-4, 9 (11)-diene-3, 20-diketone-21-acetate is used as a starting material, and the high-purity hydrocortisone is prepared through three steps of bromo-hydroxyl, debromination and hydrolysis. According to the preparation method of the high-purity hydrocortisone disclosed by the invention, the reaction process can be effectively shortened by improving the defects of a traditional process, the generation of impurities during the reaction process is controlled, the use of iodine with characteristics of high toxicity and environmental unfriendliness is avoided, the environmental pollution is reduced, and the method has characteristics of high overall conversion rate, simple operation and wide market prospect, and is suitable for industrial production.

The invention provides 3-sterone-1, 2-dehydrogenase as well as a gene sequence and application thereof. The invention discloses a gene sequence for expressing 3-sterone-1, 2-dehydrogenase, the gene sequence is shown as SEQ ID. 4, and the gene sequence is used for expression in escherichia coli. The 3-ketosterone-1, 2-dehydrogenase disclosed by the invention can be used for efficiently catalyzing androstane-4-ene-3, 17-dione (4-AD) reaction to generate androstane-1, 4-diene-3, 17-dione (ADD), and has high enzymatic activity. In addition, the soluble 3-sterone-1, 2-dehydrogenase is obtained, andthe solubility of the enzyme is improved.

The invention discloses a preparation method for a denazacort key intermediate [17alpha, 16alpha-d] methyl oxazoline steroids. The steps include: dissolving [16, 17alpha-epoxy-pregnane-20-methyl formate hydrazine acetyl-1,4-diene-3,11-diketone] in trichloromethane, adding [16, 17alpha-epoxy-pregnane-20-methyl formate hydrazine acetyl-1,4-diene-3,11-diketone] and additives into a pressure reaction kettle, leading ammonia to the reaction kettle to a certain pressure under the condition of stirring, and reacting at certain temperature; and dissolving the obtained compound crude products in glacial acetic acid, adding a certain amount of anhydride under the condition of stirring, and controlling reaction temperature. After the reaction, reaction liquid is poured into 500mL of cold 10% sodium hydroxide solution and stirred for 1 hours, and the denazacort key intermediate [17alpha, 16alpha-d] methyl oxazoline steroids is obtained after suction filtration. The method achieves safe and clean production of denazacort, is favorable for reducing environment pollution, shortens a production period, reduces production cost for enterprises, improves production safety, and is remarkable in social benefit, environment benefit and economical benefit.

The invention provides 3-sterone-1,2-dehydrogenase and an application thereof. An amino acid sequence of the 3-sterone-1,2-dehydrogenase is as shown in SEQ ID.2. The KsdD211 of the invention can catalyze a reaction of androsta-4-ene-3,17-dione (4-AD) to produce androst-1,4-diene-3,17-dione (ADD, 1,4-androstenedione), and the TLC analysis verifies the high enzymatic activity of the KsdD211. The HPLC analysis of the KsdD211catalytic reaction shows that the KsdD211 completely converts 4-AD into ADD within 18 h.

The invention relates to the technical field of biology, and provides a method for producing androstadienedione by degrading phytosterol through microorganisms. According to the invention, a new 3-sterone-1-dehydrogenase gene is cloned from Mycobacterium neoaurum DSM 1381 for the first time; through genetic engineering means, recombinant bacteria capable of efficiently expressing 3-ketosterol-1-dehydrogenase are obtained, and when the concentration of substrate phytosterol in a conversion culture medium is as high as 5g/L, the purity of the product androstadienedione in a conversion solution can be 95% or above, so that the residue of the byproduct androstenedione is effectively reduced, and the purity of the product androstadienedione is improved.

The invention relates to production methods of steroid medicine intermediates, and specifically relates to a biological dehydrogenation method of androstenedione C1 and 2 loci. The biological dehydrogenation method of the androstenedione C1 and 2 loci comprises the following steps: taking 4-androstene-3,17-dione as a substrate and simple nocardia bacterium fluid as an enzyme source, adding soybeanoil at a concentration of 100-200 ml/L and tween-80 at a concentration of 0.1-2 g/L into a transformation system, and carrying out transformation reaction at 29-31 DEG C until completion of the reaction so as to obtain a reaction product; and then, separating and purifying the reaction product so as to obtain the 1,4-androdiene-3,17-dione. On the basis of adopting a common direct conversion method, the soybean oil and the tween-80 are added according to the biological dehydrogenation method of the androstenedione C1 and 2 loci, so that conversion rate can be greatly improved that the conversion rate can be up to 96% or above; and moreover, the product is low in degradation rate, high in reaction specificity, relatively fast in conversion time and high in product quality. In addition, sterile environment is not required that only routine outdoor operation is enough; and thus, the biological dehydrogenation method of the androstenedione C1 and 2 loci is easy to operate, and suitable forindustrial large-scale production.

The invention discloses a method for synthesizing desonide impurity 11 [beta], 16 [alpha], 17 [alpha]-trihydroxypregna-1, 4-diene-3, 20-dione-21 aldehyde-16, 17-acetal acetone. The method comprises the following steps: taking desonide as an initial raw material, catalyzing by using anhydrous cupric sulfate, introducing air to oxidize, carrying out hydrolysis reaction under the catalysis of acid, and drying by using sodium sulfate to obtain the desonide impurity 11 [beta], 16 [alpha], 17 [alpha]-trihydroxypregna-1, 4-diene-3, 20-dione-21 aldehyde-16, 17-acetal acetone. The synthesis route is short, the reaction condition is mild, the impurity can be obtained without column chromatography, and the purity of the obtained impurity is 97% or above.

The present invention is compound 9beta, 11beta-epoxy-17alpha, 21-dihydroxy-16alpha-methyl-1, 4-pregnanediene-3,20-dione, as the momertasone furoate intermediate, and its production process. The intermediate 9beta, 11beta-epoxy-17alpha, 21-dihydroxy-16alpha-methyl-1, 4-pregnanediene-3,20-dione is prepared through hydrolyzing 9beta, 11beta-epoxy-17alpha, 21-dihydroxy-16alpha-methyl-1, 4-pregnanediene-3,20-dione, 21-ester (compound III) and the preparation process includes the following steps: dissolving compound III in methanol completely; dropping NaOH-MeOH solution after lowering the tempera ture to 0-5 deg.c to produce TLC tracking reaction and stopping dropping after finishing reaction; filtering and concentrating the filtrate to separate out white solid; filtering and drying to obtain the target product.

The invention provides a preparation method of a dehydroxymethasone intermediate, which comprises the following steps: by taking 21-hydroxypregna-1, 4, 9 (11), 16-tetraene-3, 20-diketone-21-acetate as a starting material, sequentially carrying out bromine hydroxylation, epoxidation, methylation and hydrolysis reaction, so as to obtain the dehydroxymethasone intermediate 9beta, 11 beta-epoxy-21-hydroxy-16 alpha-methyl progesterone-1, 4-diene-3, 20-diketone. The preparation process route provided by the invention has fewer reaction steps, the quality and yield of the product have obvious competitiveness, dangerous chemical processes are not involved, the method is green and clean, and the atom economy is improved; the preparation process has a wide industrial application prospect.

The present invention relates to a method for preparing 9β,10α-pregnane-4,6-diene-3,20-dione. The preparation method uses 9β,10α-pregnane-5,7-diene-3,20-dione diethyl diacetal (compound A) as a raw material, which is deprotected under acidic conditions to give 9β,10α-pregnane-4,7-diene-3,20-dione (compound B), which then undergoes rearrangement under alkaline conditions to give 9β,10α-pregnane-4,6-diene-3,20-dione (compound C). The method of the present invention is simple, environmentally-friendly and has a very high yield.

The invention belongs to the technical field of preparation of steroid hormone drugs, and particularly relates to a method for producing androstane dienedione by fermentation of arthrobacter simplex, which mainly comprises the following steps: optimizing fermentation culture medium components, feeding points and substrates for whole-cell transformation of arthrobacter simplex to obtain an ADD crude product with high conversion rate, and extracting and refining by mixing acetone and water to obtain the androstane dienedione. And an ADD fine product is obtained. The method effectively solves the problems that in the prior art, the conversion efficiency is not high, byproducts are difficult to separate, the process is tedious and not suitable for industrial mass production, and the like, the fermentation feeding concentration is increased to 30-60 g/L, and the conversion rate is increased to 97% or above.

The invention discloses a crystal G type of a ulipristal acetate compound (chemical name: 17alpha-acetoxy-11beta-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione, and English name: Ulipristal acetate) as well as a preparation method, a composition and applications thereof. Particularly, the invention discloses a crystal G type solid substance state form existing in the ulipristal acetate in a solid state, a preparation method of a crystal G type solid substance sample as well as applications of the ulipristal acetate crystal G type substance serving as an active pharmaceutical ingredient to preparation of medicaments for preventing pregnancy within 120h after various unprotected sexes or contraception failure and medicaments for treating metrofibroma, endometriosis, klinefelter's syndrome and glaucoma. The structural formula is as shown in the description.