- Preparation method of 1,6-didehydrogenation-17a-hydroxyl progesterone product
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The invention provides a preparation method of a 1,6-didehydrogenation-17a-hydroxyl progesterone product. The preparation method includes the steps that 1,4-androstenedione (IDD) is adopted as a raw material, firstly, IDD molecules and acetone cyanohydrin
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Paragraph 0034
(2019/05/04)
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- Method for preparing 1,6-didehydro-17a-hydroxyprogesterone product
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The invention provides a method for preparing a 1,6-didehydro-17a-hydroxyprogesterone product. The method comprises the steps that firstly soybean oil is adopted to process a by-product to obtain phytosterol, then the phytosterol is fermented to obtain ID
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Paragraph 0034
(2019/05/04)
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- Method for preparing delmadinone acetate product
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The invention provides a method for preparing a delmadinone acetate product. The method comprises the following steps: by taking IDD (1,4-Androstadienedione) as a raw material, firstly, enabling 17-site ketone in IDD molecules to react with acetone cyanohydrins in a first organic solvent under catalysis of an alkali, and introducing beta-hydroxyl and alpha-cyan into the 17-site so as to obtain hydroxyl cyanogens; preparing 1,6-bidehydrogenation-17a-hydroxyl progesterone from the hydroxyl cyanogens in the presence of methyl magnesium halide, a second organic solvent and an acid; further synthesizing a 6-site epoxy substance, further synthesizing 6-site chloride so as to obtain delmadinone, and finally carrying out 17-site esterification so as to obtain delmadinone acetate; and further carrying out heating backflow decoloring and recrystalization on the obtained delmadinone acetate with activated carbon in lower-carbon alcohol with the carbon number of smaller than 4, thereby obtaining the delmadinone acetate product. Compared with a conventional synthesis method, the method provided by the invention has multiple advantages of being simple and convenient in process operation, economic and environmental-friendly in production, high in total synthesis yield, high in product quality, low in production cost, and the like.
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Paragraph 0051; 0054-0056
(2019/03/06)
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- Delmadinone acetate preparation method
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The invention provides a delmadinone acetate preparation method which comprises the following steps: by taking 1,4-androstadienedione, that is, IDD, as a raw material, firstly, enabling 17-site ketonein IDD molecules to react with acetone cyanohydrins in a first organic solvent under catalysis of an alkali, and introducing beta-hydroxyl and alpha-cyan into the 17-site so as to obtain hydroxyl cyanogens; preparing 1,6-bidehydrogenation-17a-hydroxyl progesterone from the hydroxyl cyanogens in the presence of methyl magnesium halide, a second organic solvent and an acid; and further synthesizinga 6-site epoxy substance, further synthesizing 6-site chloride so as to obtain delmadinone, and finally carrying out 17-site esterification, thereby obtaining delmadinone acetate. Compared with a conventional synthesis method, the delmadinone acetate preparation method provided by the invention has multiple advantages of being simple and convenient in process operation, economic and environmental-friendly in production, high in total synthesis yield, high in product quality, low in production cost, and the like.
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Paragraph 0075; 0078-0080
(2019/03/06)
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- Method for preparing 1,6-bi-dehydrogenized-17a-hydroxy progesterone
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The invention provides a method for preparing 1,6-bi-dehydrogenized-17a-hydroxy progesterone. The method comprises the following steps: firstly, adopting a nutrient medium and one or more microbial strain for performing microbial fermentation on phytosterol, thereby acquiring 1,4-androstenedione, namely, IDD; taking IDD as a raw material and reacting with acetone cyanohydrins in a first organic solvent under the condition of base catalysis, thereby acquiring hydroxyl cyanide; preparing the 1,6-bi-dehydrogenized-17a-hydroxy progesterone by using the hydroxyl cyanide under the existence of methyl magnesium halide, second organic solvent and acid. Compared with the traditional production method which uses diosgenin as the raw material, the method using IDD as the raw material according to theinvention has the advantages of extensive source of raw material, economical and environment-friendly process, greatly reduced production cost, and the like; in the invention, high-cost and toxic DDQand chloranil dehydrogenating agent are no longer used; solvents used in the process are recyclable, economical, environment-friendly and beneficial to industrial production.
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Paragraph 0050; 0053-0055
(2019/04/11)
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- Preparation method of 2,6-dibromo 17a-hydroxyprogesterone
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The invention provides a preparation method of 2,6-dibromo 17a-hydroxyproxyprogesterone. The method includes the steps that 17a-hydroxyproxyprogesterone is reacted with bromine in a first organic solvent and an acid environment to obtain the dibromination product 2,6-dibromo 17a-hydroxyproxyprogesterone by making 2 and 6 sites of a 17a-hydroxyproxyprogesterone molecule subjected to dibromination,wherein a ratio of the 17a-hydroxyproxyprogesterone to the bromine to acid is 1g to (1.2 to 1.8 g) to (0.1 to 0.4 g), and a ratio of the 17a-hydroxyproxyprogesterone to the first organic solvent is 1g to (2 to 15 ml). The invention further provides a preparation method of 1,6-didehydro-17a-hydroxyproxyprogesterone correspondingly. The preparation methods of the 2,6-dibromo 17a-hydroxyproxyprogesterone and the 1,6-didehydro 17a-hydroxyproxyprogesterone have the advantages of simple and convenient process operation, safe and environment-friendly production, low production cost and the like. Compared with traditional production methods, the method has high product yield, good quality, and can reduce the product production cost by 30% to 35%; the solvent used in the process can be recovered and recycled, which is economical and environmentally friendly at the same time, and is very beneficial to industrial production.
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Paragraph 0036; 0039; 0040; 0041; 0042; 0043; 0046-0049
(2019/02/04)
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- Preparation method of 1,6-didehydro-17a-hydroxyprogesterone product
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The invention provides a preparation method of a 1,6-didehydro-17a-hydroxyprogesterone product. The preparation method comprises the following steps: firstly, enabling 17a-hydroxyprogesterone to reactwith bromine in a first organic solvent and an acidic environment to obtain a dibromide 2,6-dibromo 17a-hydroxyprogesterone; enabling the above dibromide to react with a debromination reagent in a second organic solvent for double debromination to obtain 1,6-didehydro-17a-hydroxyprogesterone; and finally, performing heating refluxing on the 1,6-didehydro-17a-hydroxyprogesterone crude product in lower alcohol under C4, and performing discoloring and recrystalization to obtain the 1,6-didehydro-17a-hydroxyprogesterone product. Compared with a traditional production method, the preparation method of the 1,6-didehydro-17a-hydroxyprogesterone product, disclosed by the invention, has the advantages of simple process operation, safe and environmentally friendly production, low production cost and the like. Compared with the traditional production method, the method is high in product yield and high in quality, and the production cost of the product can be reduced by 30 to 35 percent; the solvent used in the process can be recycled and reused, so that the method is economical, environmentally friendly and very advantageous for industrial production.
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Paragraph 0036; 0039-0042; 0047; 0049; 0054; 0056
(2019/03/28)
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- A process for preparing 1, 6 - double-dehydrogenation - 17a - hydroxy progesterone method (by machine translation)
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The present invention provides a process for preparing 1, 6 - double-dehydrogenation - 17 a - hydroxy progesterone method, said method comprises the 2, 6 - double-bromo 17 a - hydroxy progesterone such double-bromine in the 2nd organic solvent with the debromination reagent reaction double-pyrroles, to obtain the 1, 6 - double-dehydrogenation - 17 a - hydroxy progesterone; the states the debrominate reagent is lithium bromide, lithium chloride, lithium carbonate, sodium carbonate in one or more of the; double-bromine: debromination reagent=1g: 1.7 - 2.5 g, double-bromine: 2nd organic solvent=1g: 13 - 24 ml. The invention the 1, 6 - double-dehydrogenation - 17 a - hydroxy progesterone preparation method, relative to the traditional production method, with simple operation, production safety and environmental protection, low production cost and the like. The method of the invention compared with the traditional production method, the product yield is high, good quality, production cost can be reduced 30 - 35%; the solvent used in the process, can be recovered and recycled, not only economic, environmental protection, and is favorable for industrial production. (by machine translation)
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Paragraph 0034; 0037-0041; 0044-0048; 0051-0054
(2019/02/04)
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- Method for preparing 1,6-didehydro-17a-hydroxyl progesterone
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The invention provides a method for preparing 1,6-didehydro-17a-hydroxyl progesterone. The method comprises the steps: firstly, subjecting 17a-hydroxyl progesterone to a reaction with bromine in a first organic solvent in an acidic environment, and subjecting 2,6 sites of a 17a-hydroxyl progesterone molecule to dual bromination, so as to obtain a dibromide, i.e., 2,6-dibromo-17a-hydroxyl progesterone; subjecting the 2,6-dibromo-17a-hydroxyl progesterone to a didebromination reaction with a debromination reagent in a second organic solvent, thereby obtaining the 1,6-didehydro-17a-hydroxyl progesterone. Compared with the traditional production methods, the method for preparing the 1,6-didehydro-17a-hydroxyl progesterone, provided by the invention has the advantages that the process operationis simple and convenient, the production is safe and environmentally friendly, the production cost is low, and the like. Compared with the traditional production methods, the method provided by the invention has the advantages that the product is high in yield and high in quality, and the production cost of the product can be reduced by 30% to 35%; the solvents used in the process can be recovered and repeatedly applied mechanically, so that the method is economical and environmentally friendly and is very beneficial to industrial production.
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Paragraph 0035; 0038-0041; 0045-0048; 0052-0055
(2019/02/04)
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- Acetic acid cyclopropanecarboxylic progestrone dehydrogen substance a method for the synthesis of
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The invention provides a synthetic method of cyproterone acetate dehydrogenized substance, and belongs to the technical field of synthetic technologies of steroid agents. The synthetic method comprises the following processing steps of: 1) carrying out etherification reaction on 17 alpha-hydroxyl progesterone, absolute ethyl alcohol and triethyl orthoformate which serve as the raw materials, and carrying out acid-base neutralization after the reaction until reaching acidity; and 2) adding toluene to the reactant obtained in step 1) to be used as a reaction solvent; charging N2 for protecting; adding 2,3-fichloro-5,6-dicyano-1,4-benzoquinone to carry out dehydrogenation reaction; and sequentially filtering, concentrating and drying after the reaction, so as to obtain the cyproterone acetate dehydrogenized substance. According to the synthetic method, an efficient one-pot synthetic method is adopted, the double discharges in the conventional method are combined into one to be carried out, and 6s hydrogen ion in the raw materials is activated in the etherification process, so that the dual dehydrogenation reaction can be accomplished in one step, the product yield reaches 80 to 83%, the reaction period is shortened, the labor productivity is increased, the investment on equipment is decreased as well as the varieties and amount of used solvents, the environmental pollution is reduced, and the production cost of a plant is decreased.
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Paragraph 0034-0038
(2017/01/26)
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