- Synthesis method of alkyl acid testosterone
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The invention discloses a synthesis method of alkyl acid testosterone, and belongs to the technical field of synthesis and processing of medicines. The method comprises the following steps of: taking4-androstenedione (4AD) as an initial raw material, firstly, carrying out enol ether protection on the keto group at the site 3, and reducing carbonyl at the site 17 into hydroxyl; or taking 4-androstenedione (4AD) as an initial raw material, firstly carrying out enol ether protection on the keto group at the site 3, then reducing carbonyl at the site 17 into hydroxyl, then carrying out hydrolysison the site 3 to obtain testosterone, and carrying out esterification and third-site hydrolysis to obtain the testosterone ester after testosterone third-site ketal protection. According to the method disclosed by the invention, the third site is protected during esterification reaction, the generation of impurities can be reduced, and an esterification reaction solvent is a water-insoluble organic solvent, so that after the reaction is completed, products can be directly extracted in a layered manner, a large amount of water does not need to be added to separate out the products, the amountof wastewater is reduced, the solvent can be recycled, and the process is more suitable for industrial production.
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Paragraph 0033-0034; 0049-0050
(2020/12/10)
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- Method for synthesizing methyl 3-oxo-4-androstene-17beta-carboxylate
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The invention discloses a method for synthesizing methyl 3-oxo-4-androstene-17beta-carboxylate. The method comprises the following steps: (a) performing etherification protection on 3-site keto groupwith sterol fermentation broth androst-4-allyl-3,17-diketone as a starting material to obtain a compound shown by the formula 2 as shown in the specification; (b) performing Witt reaction on 3-site keto of the compound shown by the formula 2, and performing hydrolysis rearrangement to obtain a compound shown by the formula 3 as shown in the specification; and (c) performing esterification on the compound shown by the formula 3, and then collecting methyl 3-oxo-4-androstene-17beta-carboxylate shown by the formula 1 as shown in the specification from reaction products. The method disclosed in the invention has the advantages that raw material sources are stable, the pollution is less, the environmental protection is achieved and the price is low, therefore, the synthesis method is low in cost, easy, convenient and fast in process and more environmentally-friendly. The response equation is shown in the specification.
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Paragraph 0013; 0030; 0031; 0032; 0039; 0040; 0041
(2019/03/29)
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- The invention relates to a raw material synthetic stone androstenedione cholic acid (by machine translation)
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The invention discloses a high-purity stone of cholic acid synthesis method, comprises the following steps: to androstenedione as the starting material, through the 3 bit enol ether protection, wittig reaction, 3 bit vinyl alcohol the ether escapes protection, 17 site side chain addition, 3 bit carbonyl reduction, saponification reaction, seven-step reaction of catalytic hydrogenation to obtain high-purity of target substance. The method of the invention uses cheap and easily obtained androstenedione as raw materials, innovative synthetic lithocholic, simple process route, each step the reaction yield is high, and the cost is low, the large-scale production of stone cholic acid difficult problem, is suitable for industrial production. (by machine translation)
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Paragraph 0017; 0018
(2019/01/08)
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- Preparation method of canrenone intermediate
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The invention provides a preparation method of a canrenone intermediate. The preparation method comprises the following steps: taking 4-androstenedione as a substrate, adding tetrahydrofuran, p-toluenesulfonic acid and trimethyl orthoformate into the substrate, stirring the mixture until complete reaction, cooling, adding a small amount of water for a hydrolysis reaction, stirring the mixture, adding weak base solution to terminate the hydrolysis reaction, performing crystallization and filtering separation in the water, and drying, so as to obtain a compound I. In the preparation method, by optimizing reaction conditions and adding a small amount of water for a differentiation reaction after an anhydrous reaction is ended, a dual etherification phenomenon when a protection reaction is simultaneously performed on a 3-ketone group and a 17-ketone group in the prior art can be overcome, so that the purity of a product is effectively improved, the production cost is lowered, and the operation difficulty in production is lowered.
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Paragraph 0027; 0030; 0033; 0036
(2018/08/04)
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- Preparation method of melengestrol intermediate
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The invention discloses a preparation method of a melengestrol intermediate. According to the preparation method, a product compound VII, namely a melengestrol intermediate is prepared through etherification, methylenenation, cyano substitution, silicon alkoxy protection, internal nucleophilic substitution and reduction reaction of a compound 4-androstene-3,17 diketone. The used raw material 4-androstene-3,17 diketone is cheap and available. The whole process route is reasonable and optimal in design, and the synthesized product is few in impurities, good in quality, high in yield, simple in operation, mild in reaction condition, low in cost, safer and suitable for industrialization.
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Paragraph 0045; 0059; 0073; 0087; 0101; 0115
(2017/09/01)
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- Method for preparing progesterone
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The invention discloses a completely novel process route for preparing progesterone. The route adopts an initial raw material, namely 4-androstenedione (4AD) which is relatively cheap and easy to obtain, is relatively good in reaction independence of different steps, concise in procedure, simple and convenient to operate, applicable to industrial production and high in yield, and the accumulative yield of 5 steps is 55% or greater, or even up to 60%. In the situation that the price of a conventional raw material, namely 16-dehydropregnenolone acetate, soars, the process route has very high production application and economic values, and more importantly, a highly toxic reagent, namely acetone cyanohydrins, which is used in a conventional method, is not used in the method disclosed by the invention, so that the method is both economic and environmentally friendly, and is beneficial to industrial production.
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Paragraph 0038-0040
(2017/08/31)
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- A 16 ɑ-methyl steroids method for the preparation of (by machine translation)
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The invention discloses a 16 ɑ? The preparation method of compound methyl steroid race, with compound I as the starting material, through a protection reaction, nucleophilic substitution reaction, hydrolytic reaction, the 3-bit and 16 bit transformation, VI the final product is prepared. This invention uses the new starting material, the reaction step is short, on the 16 ɑ methyl steps a position which is in front of the whole product, the great convenience to have 16 ɑ methyl steroid drugs new circuit design, the follow-up all-step reaction is relatively easy to realize, high yield, which makes the production more economic, safety, more suitable for industrial production; the invention changes the existing in the industry on the format used by the reaction of methyl 16 ɑ, changes the configuration of the poor selectivity, a side reaction, and the need for a plurality of position and protect the status quo, contribute greatly to the industry the technical progress; this invention adopts the nucleophilic substituted substantially avoid the generation of the configuration isomers, almost no side reaction, greatly improving the yield, the cost is reduced. (by machine translation)
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Paragraph 0023
(2017/04/14)
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- Spironalactone process
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The present invention relates to processes for the conversion of a 3-protected steroidal 17-ketone to a 17-spiro-γ-lactone having the appropriate 17-stereochemistry for spironolactone. Novel intermediates (II, II', II", II'", IIa, IIb, IIc, IId, IIx, II'x and II"x) are also disclosed.
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