Preparation method for 3,5-estradiene-3,17beta-diacetate

A technology of diacetate and estrodiene, which is applied in the field of synthesis of 3,5-estradiene-3,17β-diacetate steroid drugs, can solve the difficulties of separation and purification, complex reactions, steroid There are many steps in drug synthesis, etc., to achieve the effect of simple process and mild conditions

Inactive Publication Date: 2017-11-21
HUBEI UNIV OF TECH
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Problems solved by technology

[0002] Steroidal drugs play an important role in the prevention and treatment of diseases, including medicine, veterinary drugs and pesticides. There are more than 400 kinds of steroidal drugs that have been marketed in foreign countries, and the existing varieties in my country account for only one-third of them, which is far from the world's advanced level

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  • Preparation method for 3,5-estradiene-3,17beta-diacetate

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Embodiment Construction

[0007] In the present invention, nandrolone, p-toluenesulfonic acid monohydrate, isopropyl acetate and No. 15 magneton are added to the reactor in sequence, and the condensed water is passed through the oil bath for heating reaction. When the system starts to condense and reflux, slowly inject Isopropenyl acetate; after the reaction, evaporate the solvent; add pyridine to the system, dropwise add isopropanol, until a white solid product is precipitated; low-temperature cooling and suction filtration, wash with cold isopropanol; collect the white solid product, After drying, the pure product of 3,5-estradiene-3,17β-diacetate can be obtained. The general reaction formula is

[0008]

[0009] Put the double-necked flask in an oil bath at 120°C to heat the reaction after passing the condensed water through the spherical condenser from bottom to top. The bottom of the double-necked flask is immersed in the silicone oil. The immersion depth is that the height of the silicone oil ...

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Abstract

The invention relates to a preparation method for 3,5-estradiene-3,17beta-diacetate. The preparation method comprises the following steps: sequentially adding nandrolone, p-toluenesulfonic acid monohydrate, isopropyl acetate and magneton No. 15 into a reactor, introducing condensed water, carrying out a heating reaction in an oil-bath pot and slowing adding isopropenyl acetate when reflux condensation of the obtained system begins; after completion of a reaction, carrying out evaporation to remove a solvent; cooling the system, adding pyridine, and adding isopropanol drop by drop until a white solid product is precipitated; carrying out low-temperature cooling and pumping filtration and then carrying out cleaning with cold isopropanol; collecting the white solid product and then carrying out drying so as to obtain a pure 3,5-estradiene-3,17beta-diacetate product. According to the invention, nandrolone is used as a substrate and a one-pot method is employed for carbonyl and hydroxyl acetylation protection so as to synthesize the product; the method is simple in process, mild in conditions and friendly to environment and has yield of up to 85%; and the synthesized product has critical application value in the fields of medicines, veterinary drugs and pesticides and is an important pro-drug for tibolone.

Description

technical field [0001] The invention relates to the synthesis of a 3,5-estradiene-3,17β-diacetate steroid drug Background technique [0002] Steroidal drugs play an important role in the prevention and treatment of diseases, including medicine, veterinary drugs and pesticides. There are more than 400 kinds of steroidal drugs that have been marketed in foreign countries, and the existing varieties in my country account for only one-third of them, which is far from the world's advanced level. There is still a certain gap in the research and development of steroid drugs compared with the advanced countries in the world. The main performance is that there are many steps in the synthesis of steroid drugs, the reaction is complicated, the long-range effect of the group is very obvious, and the yield is low. Separation and purification are difficult. The research on many steroidal drugs, especially the steroidal drugs with high technical content, is still blank in our country, and r...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0077
Inventor 张谦乐强肖祯李栋
Owner HUBEI UNIV OF TECH
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