Process for producing simvastatin ammonium salt
A technology of simvastatin ammonium salt and simvastatin acid is applied in the field of preparation of simvastatin ammonium salt, and can solve the problems of low yield in the process of ammonium salt preparation and the like
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Embodiment 1
[0025] Dissolve 8 g of simvastatin acid (compound shown in formula 1) in 120 ml of methanol solution, stir at 200 rpm at 0°C, and pass ammonia gas for about 5 minutes, check that the pH value is alkaline, stop the ammonia gas flow, stir for 10 min, and wait for Stir for half an hour after stabilization, concentrate under reduced pressure below 35°C, stop concentrating when crystals are precipitated, stir at 0°C for 2 hours, filter, and wash the crystals with methanol solution. 10.76 g of a white wet product was obtained, and vacuum-dried at 35° C. to obtain 8.04 g of simvastatin ammonium salt (compound represented by formula 2), with a yield of 96.9%.
[0026] This method can be expressed using the following procedure.
[0027]
[0028] Formula 1 Formula 2
Embodiment 2
[0030] Dissolve 8 g of compound 1 (simvastatin acid) in 100 ml of ethanol solution, stir at -15°C, pass through ammonia gas for about 5 minutes, check that the pH value is alkaline, stop passing through ammonia gas, stir at -15°C for 5 to 10 minutes, Stir for half an hour after stabilization, then concentrate under reduced pressure below 50°C, stop concentrating when crystals are precipitated, stir at -15°C for 1 hour, filter, and wash the crystals with 10ml of ethanol solution. 12.54 g of a white wet product was obtained, and vacuum-dried at 15°C to obtain 8.10 g of simvastatin ammonium salt, with a yield of 97.6%.
Embodiment 3
[0032] Dissolve 10 g of compound 1 (simvastatin acid) in 120 ml of chloroform solution, stir at 15°C, and pass through ammonia gas for about 10 minutes, check that the pH value is alkaline, stop the flow of ammonia gas, stir at 15°C for 5 to 10 minutes, and wait for stabilization After stirring for half an hour, it was then concentrated under reduced pressure at about 60°C, and the concentration was stopped after crystals were precipitated. After stirring at 15°C for 2 hours, it was filtered, and the crystals were washed with 10ml of ice-cold chloroform solution. 14.45 g of a white wet product was obtained, and vacuum-dried at 50° C. to obtain 9.91 g of simvastatin ammonium salt, with a yield of 95.5%.
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