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Method for preparing 16-dehydropregnenolone acetate by multistage filtration and recrystallization

A technology of dienol ketone acetate and recrystallization, applied in the direction of steroids, organic chemistry, etc., can solve the problem of increasing the difficulty of post-processing, unstable batch reactions, reducing product quality and product yield, and inconsistency in post-processing process changes. major problems, to achieve the effect of reducing difficulty, improving product quality and product yield, and reducing content

Inactive Publication Date: 2010-05-26
湖北民生生物医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Using diosgenin as raw material, the process of high-pressure ring-opening, oxidation, hydrolysis (elimination) extraction is very mature after decades of continuous improvement and optimization, and the yield is relatively stable, but the post-treatment process of dienolone acetate The change is not big, and the post-treatment process has become a key process that affects product quality and yield. At present, most manufacturers mainly use cyclohexane to extract the hydrolyzed product, wash it with water to neutrality, evaporate the cyclohexane to dryness, and then use ethanol The finished product is refined, and a considerable part of the dienolone acetate product with low content and the low-polarity impurities in the three-step reaction process of high-pressure ring opening, oxidation, and hydrolysis (elimination) are all left in the finished product and the mother liquor, so that it can be used cyclically , increasing the difficulty of post-processing and the instability of the next batch reaction, reducing product quality and product yield

Method used

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  • Method for preparing 16-dehydropregnenolone acetate by multistage filtration and recrystallization

Examples

Experimental program
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Embodiment 1

[0024] Throw 160kg of diosgenin, add 88kg of glacial acetic acid, 252kg of acetic anhydride, and 96kg of mother liquor. When the internal pressure reaches 0.42MP by electric heating in an open-loop tank at 194°C, turn off the power and open the loop for 50 minutes. Finally, the internal temperature reaches 208 -210°C, pressure 0.57MPa ring opening is completed. Press it into the oxidation hydrolysis tank prepared with 90kg base acid, and start to lower the temperature. When the temperature in the tank drops to 10--12°C, close the brine, and immediately add the oxidant to the oxidation tank to carry out the oxidation reaction. When the temperature rose to 98°C, the reaction was timed for 25 minutes, and then steam was introduced into the jacket to heat up the reaction, and the acetic acid was recovered by distillation under normal pressure for 50 minutes, and then the glacial acetic acid was recovered under reduced pressure for 30 minutes. After the reaction is completed, the f...

Embodiment 2

[0026] The method for producing monoenolone acetate by multi-stage filtration and recrystallization, throws 160kg of sisal saponin, adds 88kg of glacial acetic acid, 252kg of acetic anhydride, and 96kg of mother liquor, and heats up in an open-loop tank at 194°C with an internal pressure of 0.42MP. a, power off timing. Open the ring for 50 minutes, and finally the internal temperature reaches 208-210°C, and the pressure is 0.57MPa to complete the ring opening. Press it into the oxidation hydrolysis tank prepared with 90kg base acid, and start to lower the temperature. When the temperature in the tank drops to 10--12°C, close the brine, and immediately add the oxidant to the oxidation tank to carry out the oxidation reaction. When the temperature rose to 98°C, the reaction was timed for 25 minutes, and then steam was introduced into the jacket to heat up the reaction, and the acetic acid was recovered by distillation under normal pressure for 50 minutes, and then the glacial ac...

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Abstract

The invention relates to a method for preparing 16-dehydropregnenolone acetate by multistage filtration and recrystallization, comprising the following steps of: high-pressure ring-opening (cracking), oxidizing, hydrolyzing and extracting, multistage filtering after posttreatment, recrystallizing and refining, recovering and applying mother liquor, and the like. In the method, by multistage filtration and recrystallization technologies the contents of most 16-dehydropregnenolone acetate product with low content and low-polarity impurities in the reaction processes of high-pressure ring-opening, oxidizing and hydrolyzing in the finished product and the mother liquor are reduced, therefore, the posttreatment difficulty is reduced, the stability of the next-batch reaction is increased, and the product quality and the product yield are improved.

Description

technical field [0001] The invention belongs to the technical field of production of steroid hormone intermediates, and in particular relates to a method for producing dienolone acetate. Background technique [0002] Dienolone acetate (referred to as diene) chemical name: 5.16-pregnadiene-3β-ol-20-one acetate, molecular formula is C 23 h 32 o 3 , which has the parent nucleus of cyclopentane-perhydrophenanthrene, which is a typical steroid compound. Diene is an important intermediate in the synthesis of various steroid hormone drugs, which can be used as raw materials to produce sex hormone drugs (such as acetylene, progesterone, methyl testosterone), adrenocortical hormones (such as hydrocortisone, prednisone, dexamethasone, betamethasone) etc. At present, the industrial production of dienolone acetate is mainly semi-synthesized from steroidal compounds obtained from natural resources. The raw materials for the synthesis of dienolone acetate include diosgenin and steroid...

Claims

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Application Information

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IPC IPC(8): C07J13/00
Inventor 陈孝华
Owner 湖北民生生物医药有限公司
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