Method for preparing 9 beta, 10 alpha-dehydroprogesterone diethyl diketal by utilizing LED light source

A technology of ketone diethylene ketal and LED light source, which is applied in the direction of ketal steroids, chemical instruments and methods, steroids, etc., can solve the problems of complex photochemical reaction products and difficult processes, and achieve important economic and social values. The effect of less control points and easy operation

Active Publication Date: 2020-02-14
GUANGXI NORMAL UNIV
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  • Claims
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AI Technical Summary

Problems solved by technology

[0012] The object of the present invention is to use 9α, 10β-dehydroprogesterone diethylene ketal as raw material to prepare the key intermediate of dydrogesterone in the photochemical reaction through photochemical reaction, because the photochemical reaction product is relatively complicated due to the use of mercury lamp as the light source , the process is not easy to enlarge and other defects, using LED light source with a single wavelength to carry out photochemical reaction, providing a high total yield, green environmental protection, simple operation, easy to scale up using LED light source to prepare 9β, 10α - dehydroprogesterone diethyl Diketal method

Method used

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  • Method for preparing 9 beta, 10 alpha-dehydroprogesterone diethyl diketal by utilizing LED light source
  • Method for preparing 9 beta, 10 alpha-dehydroprogesterone diethyl diketal by utilizing LED light source
  • Method for preparing 9 beta, 10 alpha-dehydroprogesterone diethyl diketal by utilizing LED light source

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Experimental program
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Effect test

Embodiment 1

[0043] Dissolve 10 grams of the raw material 9α, 10β-dehydroprogesterone diethylenediketal in 1 L of reaction solvent methanol, place it in the feeding tank and cool it to -30°C, protect it with argon, open the first photochemical reactor, the second Two photochemical reactors and condensing systems. The photochemical ring-opening reaction is carried out in the first photochemical reactor, and the photochemical ring-closing reaction is carried out in the second photochemical reactor. The wavelength of the LED light source in the first photochemical reactor is 270 nanometers, and the second photochemical The wavelength of the LED light source in the reactor is 330 nanometers, then the flowmeter is turned on, and the reaction temperature is controlled at -30±5°C.

[0044] The raw material solution passes through the first photochemical reactor to obtain a solution after the ring-opening reaction, and then directly enters the second photochemical reactor to obtain a solution conta...

Embodiment 2

[0047] Reaction temperature is controlled at-15 ± 5 ℃, and other conditions are with embodiment 1.

[0048] The reaction time is about 4 hours, and the HPLC test results show that the content of the raw material 9α, 10β-dhydroprogesterone diethylene ketal in the crude product is about 30%, and the content of the target product 9β, 10α-dhydroprogesterone diethylene ketal About 62%, other impurity content about 8%.

Embodiment 3

[0050] Reaction temperature is controlled at 0 ± 5 ℃, and other conditions are with embodiment 1.

[0051] The reaction time is about 3.5 hours, and the HPLC test results show that the content of the raw material 9α, 10β-dehydroprogesterone diethylene ketal in the crude product is about 38%, and the content of the target product 9β, 10α-dehydroprogesterone diethylene ketal About 56%, other impurity content about 6%.

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Abstract

The invention discloses a method for preparing 9 beta, 10 alpha-dehydroprogesterone diethyl diketal by utilizing an LED light source. According to the method, 9 alpha, 10 beta-dehydroprogesterone diethyl diketal is taken as a raw material; the LED light source with a single wavelength is used for carrying out photochemical reaction; so that dydrogesterone key intermediate 9 beta, 10 alpha-dehydroprogesterone diethyl diketal is prepared, the defects in the prior art that when a mercury lamp is used as a light source, photochemical reaction products are complex, the process is not easy to amplify and the like are avoided, and the method which is high in total yield, environmentally friendly, easy and convenient to operate and easy to amplify is provided.

Description

technical field [0001] The invention relates to the technical field of photochemical synthesis, in particular to a method for preparing 9β, 10α-dehydroprogesterone diethylenediketal by using an LED light source. Background technique [0002] Dydrogesterone (Dydrogesterone) is widely used in miscarriage protection, miscarriage prevention and treatment of various diseases caused by endogenous progesterone deficiency. It was launched in the world in 1961 and sold in more than 150 countries. Abbott in the United States can produce it. 9β,10α-dehydroprogesterone diethylene ketal 1, also known as diethylene ketal of 9β,10α-pregna-4,6-diene-3,20-dione, is a synthetic dydrogesterone The key intermediate of , its structural formula is as follows. [0003] [0004] At present, there is no mature technology for industrialized preparation of 9β, 10α-dhydroprogesterone diethylenediketal in China, so dydrogesterone has not yet been successfully imitated. [0005] The currently discl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J21/00
CPCC07J21/006
Inventor 潘成学苏桂发于成龙李永怡杨倩方淑君
Owner GUANGXI NORMAL UNIV
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