- Efficient preparation method of delta-canrenone
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The invention discloses an efficient preparation method of delta-canrenone, and belongs to the technical field of preparation of intermediates of medicines. The method comprises the following steps of: by taking 9 alpha-hydroxyl-4-androstenedione as a raw material, firstly removing 9-site hydroxyl through dehydration reaction to generate delta double bonds, then protecting 3-site carbonyl, then performing epoxidation on 17-site carbonyl, condensing with malonic acid diester to form a lactone ring, and performing oxidative decarboxylation or decarboxylation oxidation reaction to obtain delta-canrenone. According to the method, the raw materials are cheap and easy to obtain, the cost is low, reaction products in all steps are easy to purify, the total mass yield of the final product is higher than 80%, and the method is high in operability, extremely high in commercial competitiveness, suitable for industrial large-scale production and good in economic benefit.
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Paragraph 0034; 0036
(2020/12/31)
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- A pregna - 1, 4, 9 (11), 16 (17) - tetraene - 3, 20 - dione synthetic method and intermediate
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The invention relates to a synthesis method and main intermediates of pregnene-1,4,9 (11),16 (17)-tetraenol-3, 20-diketone. The synthesis method sequentially comprises the following steps of reacting a second intermediate and tosylmethyl isocyanide in an organic solvent at the temperature of lower than 35 DEG C below zero to generate a third intermediate; reacting the third intermediate and a methylated reagent in an organic solvent at the temperature of 70-90 DEG C, and then, removing methyl ether protecting groups and tosylmethyl isocyanide under the action of an acid to obtain a fourth intermediate; and reacting the fourth intermreidate under the action of 3-ketosteroid-1-dehydrogenase to generate pregnene-1,4,9 (11),16 (17)-tetraenol-3, 20-diketone. Raw materials of pregnene-1,4,9 (11),16 (17)-tetraenol-3, 20-diketone are cheap and available; the yield of pregnene-1,4,9 (11),16 (17)-tetraenol-3, 20-diketone is relatively high; a C17-position side chain is introduced by using tosylmethyl isocyanide, so that acetone cyanohydrin serving as a highly-toxic reagent is prevented from being used; and the synthesis method is safe, environment-friendly and suitable for industrial production.
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Paragraph 0030; 0031; 0032; 0033
(2017/08/25)
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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 0028
(2017/04/14)
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- Method for preparing tetraene acetate and derivatives thereof
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The invention relates to a method for preparing tetraene acetate and derivatives thereof. The method comprises the steps of obtaining a compound II through etherification reaction of a compound I and an etherification agent in the atmosphere of protective gases, obtaining a compound III through addition reaction of the compound II and a reagent A under the action of strong base and hydrolysis and elimination reaction of the compound II and the reagent A in the presence of an acid solution, obtaining a compound IV through substitution reaction and rearrangement reaction of the compound III and acetate, and conducting 1 position dehydrogenation and 2 position dehydrogenation on the compound IV to obtain the tetraene acetate and derivatives thereof. According to the method, the compound I is taken as the raw material and subjected to carbonyl etherification, addition, hydrolysis, elimination, rearrangement and dehydrogenation reaction to obtain the product, the raw material compound I is easy to obtain, cost is low, no precious metal is needed during preparation, reaction conditions are easy to control, operation is convenient, the method is suitable for large-scale industrial production, and the obtained tetraene acetate is an important intermediate for synthesis of dexamethasone, budesonide, betamethasone and other steroidal drugs.
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Paragraph 0117
(2016/12/01)
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- 17 α-chloroethynyl pregnane derivatives
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Known pregnane derivatives are prepared by esterificiation of known androstane derivatives to give new ester of Formula III STR1 wherein in each case symbolizes a single bond or a double bond, n is 1 or 2, R1 is hydrogen or methyl, R2 is hydrogen or formyl, and R3 is chlorine, hydroxy or an alkanoyloxy group of up to 6 carbon atoms, and reaction of the latter with Ag(I) and formic acid.
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