Potassium Carbonate → 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-1,2,3-triazolo(4,5-d)pyrimidin-3-yl)tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxol-4-yl)oxy)ethanol

Participants

Reaction Steps

trans-(1R,2S)-2-(3,4-Difluorophenyl)cyclopropanaminium (2R)-2-hydroxy-2-phenylethanoate (146 kg, prepared as described in WO2008/018822, WO2008/018823, WO01/92200) and potassium carbonate (156 kg) were dissolved in water (576 kg) and charged to the 2-({(3aR,4S,6R,6aS)-6-[7-Chloro-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl]-2,2-dimethyltetrahydro-3 aH-cyclopenta[d][1,3]dioxol-4-yl}oxy)ethanol solution with a rate that kept the temperature of the reaction ≦30° C. After the conversion criterion was reached (>99%) the water layer was separated off. The organic layer was washed twice with acetic acid (18 kg) and sodium chloride (13 kg) in water (560 kg) and then twice with sodium chloride (54 kg) in water (438 kg), whereafter the organic layer was used in the next step.

Provenance & Evidence