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Process for synthesizing 3-acetoxy-9 beta, 10 alpha-pregna-5, 7-diene-20-ketone

A technology of acetoxy and synthetic methods, applied in the field of chemical drug intermediates of dehydroprogesterone, can solve problems such as large safety hazards, difficult industrial production, low light conversion rate, etc., achieve reduced emissions, mild reaction conditions, The effect of high yield

Inactive Publication Date: 2008-12-10
台州市万福制药有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the light conversion rate is low, so that the yield of this step is only 10.62%. The solvent used in the photochemical reaction is tetrahydrofuran, and a large amount of ether is used in the post-treatment, which has a large safety hazard and is difficult to form industrial production.

Method used

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  • Process for synthesizing 3-acetoxy-9 beta, 10 alpha-pregna-5, 7-diene-20-ketone
  • Process for synthesizing 3-acetoxy-9 beta, 10 alpha-pregna-5, 7-diene-20-ketone

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Effect test

Embodiment 1

[0025] Dissolve 10kg of 3-acetoxy-pregna-5,7-dien-20-one in 1000L ethanol, flow through a quartz reactor, select a light source with a wavelength of 275-295nm, and irradiate with ultraviolet light for 5 hours to obtain a suitable After the product is produced, its solution is added to the photosensitizer anthracene, and the amount of anthracene in the solution is controlled at 0.01g / L, and flows through 10m 2 Quartz three-dimensional coil with a diameter of 1cm is irradiated in an irradiator with an external fluorescent lamp with a wavelength of 300-313nm, the flow rate is controlled at 1000mL / min, and the irradiation temperature is 0-20°C. The irradiated solution flows into the concentration tank and is concentrated to dryness under reduced pressure. The residue in the tank is dissolved with 100L toluene, the insoluble matter (unreacted raw materials) is filtered off, the filtrate is concentrated to dryness under reduced pressure, and 300L acetone and an appropriate amount of ...

Embodiment 2

[0027] Dissolve 10kg of 3-acetoxy-pregna-5,7-dien-20-one in 2000L ethanol, flow through a quartz reactor, select a light source with a wavelength of 275-295nm, and irradiate with ultraviolet light for 4 hours to obtain a suitable After the product is produced, its solution is added to the photosensitizer anthracene. The amount of anthracene in the solution is controlled at 0.5g / L, and the flow through 10m 2 Quartz three-dimensional coil with a diameter of 1cm is irradiated in an irradiator with an external fluorescent lamp with a wavelength of 300-313nm, the flow rate is controlled at 1500mL / min, and the irradiation temperature is 0-20°C. The irradiated solution flows into the concentration tank and is concentrated to dryness under reduced pressure. The residue in the tank is dissolved with toluene, and the insoluble matter (unreacted raw materials) is filtered off. minutes, filtered, concentrated, crystallized by cooling, centrifuged, and dried to obtain 3.2 kg of 3-acetoxy-9...

Embodiment 3

[0029] With reference to the process steps of Example 1, the difference is that 10 kg of the raw material 3-acetoxy-pregna-5,7-dien-20-one is dissolved in 1500L ethanol, and the amount of the solution added to the photosensitizer anthracene solution is controlled at 0.2 g / L, control flow 1200mL / min, 3.5kg yield 35%.

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Abstract

The invention relates to a method for synthesizing 3-acetoxy-9 beta, 10 alpha-pregna-5, 7-diene-20-ketone. 3-acetoxy-pregna-5, 7-diene-20-ketone is used as a raw material to synthesize the 3-acetoxy-9 beta, 10 alpha-pregna-5, 7-diene-20-ketone. The method is characterized in that: the method adopts a two-step method of photocatalytic reaction; in the first step of the photocatalytic reaction, light waves with a wavelength of between 275 and 295 nm are selected; and in the second step of the photocatalytic reaction, light waves with a wavelength of between 300 and 313 nm are selected and added with photosensitizer anthracene. The method has the advantages of readily available raw materials, mild reaction condition, high yield, low cost, good product quality, etc.

Description

Technical field [0001] The invention relates to a chemical drug intermediate of dehydroprogesterone, in particular to a synthesis method of 3-acetoxy-9β, 10α-pregna-5,7-dien-20-one. Background technique [0002] Compound 3-acetoxy-9β, 10α-pregna-5,7-dien-20-one is a synthetic dehydroprogesterone (also known as dydrogesterone, 6-dehydroreverse progesterone, chemical name: 9β , an important intermediate of 10α-pregna-4,6-diene-3,20-dione). [0003] The Royal Netherlands Chemical Society (1960, 79, P771) reported that Solvay Pharmaceutical Company of the Netherlands produced the raw material drug of dehydroprogesterone products, and the process route adopted was: using the by-product of vitamin D production-photosterol to be oxidized by Wo Shi , rearrangement, lithium ammonia reduction, ozonation, 20-position complexation, oxidation, dehydrogenation and other chemical reactions to obtain dehydroprogesterone products, with a total yield of about 3%. The disadvantage is that the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00
Inventor 陆志仁王锦理王建江张雪
Owner 台州市万福制药有限公司
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