반응 #309704

반응 방정식

Rosuvastatin tert-butyl ester

NaOH

→

rosuvastatin sodium

수율 100.0%

용매

THF water

반응 조건

후처리

1. 1
   기타giving a clear yellow solution
2. 2
   기타Then THF is removed completely under the reduced pressure (20 mbar) at 40° C
3. 3
   workup.ADDITIONThe remaining aqueous solution is diluted with water to 25 mL
4. 4
   세척washed with AcOEt (2×10 mL)
5. 5
   기타After separation from the organic layer aqueous phase
6. 6
   workup.DISTILLATIONis distilled under the reduced pressure (20 mbar) at 40° C.
7. 7
   기타to completely remove the dissolved AcOEt
8. 8
   workup.ADDITIONThe remaining clear solution of sodium rosuvastatinate is diluted with water to 25 mL

실험 절차

Rosuvastatin tert-butyl ester (3.0 g, 5.6 mmol) is dissolved in 25 mL of a 4:1 mixture of THF/water. The clear solution is warmed to 30° C. and 8.0 M NaOH (0.75 mL, 6.0 mmol) was added portionwise. The reaction mixture is stirred at 30° C. for 2 hours giving a clear yellow solution. Then THF is removed completely under the reduced pressure (20 mbar) at 40° C. The remaining aqueous solution is diluted with water to 25 mL and washed with AcOEt (2×10 mL). After separation from the organic layer aqueous phase is distilled under the reduced pressure (20 mbar) at 40° C. to completely remove the dissolved AcOEt. The remaining clear solution of sodium rosuvastatinate is diluted with water to 25 mL and liophylized to afford 2.81 g (100%) of rosuvastatin sodium salt as white powder.

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