Water → Rosuvastatin

Participants

Reaction Conditions

Reaction Steps

A 800 cm3 autoclave is charged with 16.1 g (0.03 mol) of rosuvastatin n-butylamide, 644 cm3 of water 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 residue is stirred in the mixture of tert-butylmethylether and heptane (2:5, v/v) and the crystals are filtered. Thus 16.2 g (99%) of rosuvastatin TBA salt are obtained. The crude salt is boiled in acetonitrile/2-propanol (8.6:1, v/v) mixture, subsequently further stirred at room temperature, filtered, washed and dried. The product thus obtained is boiled in acetonitrile, 2-propanol is added to the boiling mixture, decolorized with carbon and filtered. The precipitated crystals are filtered and washed with acetonitrile. Yield 10.9 g (66%) rosuvastatin TBA salt having the purity (as determined by high-performance liquid chromatography, HPLC) exceeds 99.5%.

Provenance & Evidence