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Refining method of didrogesterone

A refining method and technology of dydrogesterone, applied in the direction of steroids, organic chemistry, etc., can solve the problems that peroxides are easy to be dangerous and difficult to remove.

Active Publication Date: 2022-02-18
HUNAN KEREY BIOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is that there are huge safety hazards, and the treatment of peroxides in the production process is prone to danger; the other is that under the action of strong oxidants, dydrogesterone products may be oxidized, thereby introducing new impurities, which are more difficult to remove

Method used

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  • Refining method of didrogesterone
  • Refining method of didrogesterone
  • Refining method of didrogesterone

Examples

Experimental program
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Effect test

Embodiment 1

[0025]

[0026] 20g crude dydrogesterone (purity 94.9%, aldehyde impurity content 2.1%, see figure 1 ) into the reaction bottle with magnetron, add 100mL of dichloromethane and stir to dissolve, add 40mL of water, 6g of sodium bisulfite, continue to stir vigorously, insert the ultrasonic launch rod of the ultrasonic reflector below the liquid level, and start the ultrasonic reaction The instrument was stirred at room temperature (25-30 °C) for 2 h. Pour out the reaction solution, let stand for stratification, and separate the layers. Add 50 mL of water to the organic layer, stir to separate the layers, add 50 mL of water again, concentrate dichloromethane to dryness, add acetone to recrystallize, crystallize at -5 to 0 °C, and filter, Dried dydrogesterone fine product, the purity is 99.84%, the sum of the content of aldehyde group impurity 1 and impurity 2 is less than 0.1%, specifically 0.072%, see figure 2 .

Embodiment 2

[0028] 20g crude dydrogesterone (purity 94.93%, aldehyde group impurity content 2.1%) was added to a reaction flask with a magnet, 100mL of dichloromethane was added and stirred to dissolve, 50mL of water and 6g of sodium metabisulfite were added, and vigorous stirring was continued. Insert the ultrasonic transmitting rod of the reflector below the liquid level, turn on the ultrasonic reactor, and stir for 2 hours at room temperature (25-30°C). Pour out the reaction solution, let stand for stratification, separate the layers, add 50 mL of water to the organic layer, stir to separate the layers, add 50 mL of water again, concentrate dichloromethane to dryness, add acetone for recrystallization, crystallize at -5 to 0 °C, filter, The fine dydrogesterone is obtained by drying, the purity is 99.82%, and the sum of the content of aldehyde group impurity 1 and impurity 2 is less than 0.1%.

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Abstract

The invention provides a method for refining didrogesterone, which comprises the following steps of: reacting a didrogesterone crude product with a sulfite derivatization reagent in the presence of an organic solvent and under an ultrasonic condition, so that an aldehyde group impurity as shown in a formula I is derivatized and dissolved in water to be removed, and a didrogesterone refined product is obtained. The invention provides the environment-friendly, safe, simple and convenient method for removing the aldehyde impurity, so that the content of the aldehyde impurity I in the crude product didrogesterone is reduced to 0.1% or below, which meets the pharmacopoeia standard and is higher than the industrial standard.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis / drug synthesis, in particular to a method for refining dydrogesterone. Background technique [0002] Dydrogesterone, also known as dehydroprogesterone, has a chemical name of 9β,10α-pregna-4,6-diene-3,20-dione, CAS number: 152-62-5. The chemical formula of dydrogesterone is as follows: [0003] [0004] Dydrogesterone is widely used not only for preventing miscarriage and preventing miscarriage, but also for treating various diseases caused by insufficient endogenous progesterone, such as dysmenorrhea, endometriosis, secondary amenorrhea, irregular menstrual cycle , dysfunctional uterine bleeding, premenstrual syndrome, threatened or habitual abortion due to progesterone deficiency, infertility due to luteal insufficiency, etc. There are currently two dosage forms of Duphaston (Dydrogesterone Tablets) and Femoston (Femoston Estradiol Tablets / Estradiol Dydrogesterone Tablets...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J7/00
CPCC07J7/002Y02P20/55
Inventor 唐杰龙能吟刘靖周桑
Owner HUNAN KEREY BIOTECH
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