Preparation method of 17[alpha]-hydroxyprogesterone

A hydroxyprogesterone and activated carbon technology, applied in steroids, organic chemistry and other directions, can solve the problems of long reflux decolorization time and slow activated carbon reaction, and achieve the effect of shortening the time, increasing the reaction rate and reducing the production cost.

CN112898367AInactive Publication Date: 2021-06-04HEBEI JINSHUI BIOTECHNOLOGY CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2021-06-04
Estimated Expiration
Not applicable · inactive patent
Patent Text Reader

Abstract

The invention discloses a preparation method of 17[alpha]-hydroxyprogesterone, wherein the preparation method comprises the steps: refining: step 1, dissolving 1 W of a crude product into a mixed solution of 4-5 V dichloromethane and 6-8 V ethanol, and heating to dissolve the crude product; step 2, weighing activated carbon exceeding a preset amount, then putting the activated carbon into a drying device for drying, controlling the drying temperature to be 60-85 DEG C, and controlling the drying time to be 10-15 minutes; and step 3, taking out the activated carbon dried in the step 2, and then placing the activated carbon in a grinding device for fine grinding. According to the scheme, activated carbon in the refining process in an original scheme is finely processed and then added, so that the reaction rate is effectively increased, the time of reflux decoloration is shortened, large-scale production and processing are facilitated, and the production cost is further reduced.
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Description

Technical field

[0001] The present invention relates to the preparation of steroidal hormone drug intermediates, and more particularly to a 17α-hydroxy progesterone preparation method. Background technique

[0002] 17α-hydroxybatidone is an important intermediate for producing steroid hormones, in which an intermediate can produce anteenum progesterone, acetate hydrochloride, chlorine progesterone and other progesterone and predenzone, aplastic Corticoids such as acetic acid, which can be seen in the steroidal market. It is very vast demand, and the starting material of 17α-hydroxybone ketone is currently replaced by 4-ounced (4AD). Ethylene, since the olefin is a raw material with potato saponin, a hemp saponin, and a reaction, an open loop, acetylation, oxidation, hydrolysis, epoxidation, oxidation, addition, catalytic hydrogenation, and other reactions. . This traditional preparation method has a severe environmental pollution, the synthesis step is cumbersome, the process is ...

Examples

Embodiment 1

[0023] In this embodiment, a 17α-hydroxy progesterone preparation method is proposed, including the following steps:

[0024] refined:

[0025] Step 1: The crude product 1 W is dissolved in 4 to 5 V dichloromethane and 6 to 8V ethanol mixed, heat it to dissolve;

[0026] Step 2: The activated carbon is performed extends over the predetermined amount, which is then placed in the drying apparatus for drying, and the drying temperature is controlled at 60 to 85 ° C, the drying time is controlled at 10-15 min;

[0027] Step 3: Remove the activated carbon after drying in step 2, then placed in the abrasive device for fine grinding;

[0028] Step 4: Collect and screen the active carbon ash refined in step 3, and perform a precision weighing, screen 0.05W.

[0029] Step 5: The filtered active carbon ash, refluxed 0.3 hours, concentrated from about 90% of the solvent, cooling 10 ° C to filter, dry below 70 ° C, product grade 17a-hydroxy progesterone, obtained product HPLC detection conten...

Embodiment 2

[0035] In this embodiment, a 17α-hydroxy progesterone preparation method is proposed, including the following steps:

[0036] refined:

[0037] Step 1: The crude product 1 W is dissolved in 4 to 5 V dichloromethane and 6 to 8V ethanol mixed, heat it to dissolve;

[0038] Step 2: The activated carbon is performed extends over the predetermined amount, which is then placed in the drying apparatus for drying, and the drying temperature is controlled at 60 to 85 ° C, the drying time is controlled at 10-15 min;

[0039] Step 3: Remove the activated carbon after drying in step 2, then placed in the abrasive device for fine grinding;

[0040] Step 4: Collect and screen the active carbon ash refined in step 3, and perform a precision weighing, screen 0.05W.

[0041] Step 5: The filtered active carbon ash, refluxed 0.4 hours, concentrated from about 90% of the solvent, cooling below 10 ° C to filter, dry below 70 ° C, product grade 17a-hydroxy progesterone, obtained product HPLC detection ...

Embodiment 3

[0047] In this embodiment, a 17α-hydroxy progesterone preparation method is proposed, including the following steps:

[0048] refined:

[0049] Step 1: The crude product 1 W is dissolved in 4 to 5 V dichloromethane and 6 to 8V ethanol mixed, heat it to dissolve;

[0050] Step 2: The activated carbon is performed extends over the predetermined amount, which is then placed in the drying apparatus for drying, and the drying temperature is controlled at 60 to 85 ° C, the drying time is controlled at 10-15 min;

[0051] Step 3: Remove the activated carbon after drying in step 2, then placed in the abrasive device for fine grinding;

[0052] Step 4: Collect and screen the active carbon ash refined in step 3, and perform a precision weighing, screen 0.05W.

[0053] Step 5: The filtered active carbon ash, refluxed 0.5 hours, concentrated from about 90% of the solvent, cooling 10 ° C to filtration, 70 ° C, drying, product grade 17a-hydroxypertone, obtained product HPLC detection content> 9...