Tert-Butylamine → Rosuvastatin

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

An autoclave having 800 cm3 volume is charged with 16.1 g (0.03 mol) of rosuvastatin n-butylamide, 644 cm3 of water/ethanol (9:1, v/v) solvent mixture and 43.9 g (63.3 cm3; 0.60 mol) tert-butylamine. The reaction mixture is stirred for 24 hours at 120° C. The mixture is allowed to cool to room temperature, diluted with 2-propanol and evaporated in vacuo. The evaporation residue is stirred in the mixture of tert-butylmethylether and heptane (2:5, v/v) and the crystals are filtered. Thus 16.7 g (100%) of rosuvastatin TBA salt are obtained. The crude salt is boiled in the mixture of acetonitrile and 2-propanol (8.6:1, v/v), stirred at room temperature, filtered, washed and dried. The product thus obtained is boiled in acetonitrile, 2-propanol are added to the boiling mixture, decolorized with carbon and filtered. The precipitated crystals are filtered and washed with acetonitrile. In this way 10.7 g (64%) of rosuvastatin TBA salt having a purity (as determined by HPLC) greater than 99.5% are obtained.

Herkunft & Nachweise