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.
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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...
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Abstract
Description
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