Medroxyprogesterone Acetate synthesis
- Product Name:Medroxyprogesterone Acetate
- CAS Number:71-58-9
- Molecular formula:C24H34O4
- Molecular Weight:386.52
32634-95-0
71-58-9
S1: To a 500 mL three-necked flask was added 40 g of 6-methylenepregna-4-en-17α-ol-3,20-dione-17-acetate, 400 mL of ethanol, 30 g of cyclohexene and 2.5 g of 5% palladium-carbon catalyst. The reaction mixture was heated to 75-78 °C and maintained for 5 hours. The reaction process was monitored by HPLC. Upon completion of the reaction, the reaction mixture was filtered to recover the palladium-carbon catalyst.S2: After the reaction solution was cooled to below 50 °C, 14 mL of hydrochloric acid was slowly added and the reaction temperature was controlled between 40-50 °C for 3 hours. At the end of the reaction, the pH of the reaction solution was adjusted with saturated sodium bicarbonate solution to 6-7. Subsequently, the reaction solution was concentrated to a paste under reduced pressure and the temperature inside the flask was lowered to below 20 °C. The reaction solution was then dried to a solid of 0.5 mL. The resulting solid was filtered, washed and dried to give 28.5 g of crude product.S3: The crude product was recrystallized using a solvent mixture of methanol and dichloromethane to give 35 g of pure product with a total yield of 87.5% and an impurity F content of 0.35%.
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Yield:71-58-9 87.5%
Reaction Conditions:
with ethanol;5%-palladium/activated carbon in cis-cyclohexene at 75 - 78; for 5 h;Reagent/catalyst;Temperature;
Steps:
3 Example 3 An medroxyprogesterone acetate preparation method includes the following steps
S1: 40 g of 6-methylenepregn-4-ene-3,20-dione-17α-acetate, 400 ml of ethanol, 30 g of cyclohexene, and 2.5 g of 5% palladium-carbon were placed in a 500 ml three-neck flask. The reaction was heated to 75-78°C for 5 hours. The reaction was monitored by HPLC. After the reaction was complete, the palladium carbon in the reaction solution was filtered and recovered.S2: After the temperature of the reaction solution is lowered to below 50°C, 14 ml of hydrochloric acid is added, and the reaction is incubated at 40-50°C for 3 hours. After the insulation is completed, the pH of the reaction solution is adjusted to pH 6-7 with a saturated sodium bicarbonate solution, and then the temperature in the flask is reduced to below 20°C when the atmospheric pressure is concentrated to a paste. The material is filtered, washed and dried to obtain safety. Methedrone crude product 28.5g;S3: Recrystallization from a mixed solvent of methanol and methylene chloride gives an ampoule ketone 35 g with a total yield of 87.5% and an impurity F content of 0.35%
References:
CN107573395,2018,A Location in patent:Paragraph 0012; 0028; 0033; 0036-0040
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