Synthetic method of spironolactone
A synthesis method and spironolactone technology, applied in the field of chemical synthesis, can solve problems such as irritating odor of thioacetic acid, unfavorable sustainable development, high environmental protection pressure, etc., and achieve the effects of good economic value, beneficial to sustainable development, and easy operation.
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Embodiment 1
[0022] 12.25 g canrenone, 9.5 g oxalic acid, 6.2 g potassium thioacetate and 100 ml ethanol were added to the reaction vessel. Heat to reflux reaction for 3 hours, add 2.4g potassium thioacetate, and continue reflux reaction for 2 hours. After the reaction is completed, stop heating, cool down to -10°C, keep warm for 2 hours, filter, and filter cake with 10ml water and Rinse with 10ml of ethanol, dry to obtain 13.8g of crude product, and recrystallize with ethanol to obtain 12.25g, the total yield is 75%, HPLC99.2%.
Embodiment 2
[0024] Add 12.25g canrenone, 8.6g potassium thioacetate and 100ml ethanol into the reaction vessel, heat to reflux, slowly add 9.5g oxalic acid dropwise for 1 hour, and continue to react for 3 hours after the addition. After the reaction, stop heating, cool down to -10°C, keep warm for 1.8 hours, filter, filter cake with 10ml of water and 10ml of ethanol, and dry to obtain 13.5g of crude product, then recrystallize with ethanol to obtain 12.36g, The total yield is 75.8%, and the HPLC purity is 99.3%.
Embodiment 3
[0026] 12.25 g of canrenone, 8.6 g of potassium thioacetate and 100 ml of ethanol were added to the reaction vessel. Heat to reflux, slowly add 7.3g methanesulfonic acid dropwise for about 1 hour, and continue to react for 3 hours after the addition is complete. After the reaction is complete, stop heating, cool down to -10°C, keep warm for 2.2 hours, filter, filter the cake with 10ml of water and 10ml of ethanol, and dry to obtain 14.5g of crude product, which is then recrystallized with ethanol to obtain 12.43g , The total yield is 76%, and the HPLC purity is 99.0%.
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