Medroxyprogesterone Acetate synthesis
- Product Name:Medroxyprogesterone Acetate
- CAS Number:71-58-9
- Molecular formula:C24H34O4
- Molecular Weight:386.52
32634-95-0
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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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