反应详情

温度

5 °C

Nilotinib base (0.300 g, 0.57 mmol) was dissolved in TFE (2 mL) at 40° C. to obtain a mixture. The mixture was stirred and added to a solution of citric acid (0.218 g, 1.13 mmol) in TFE (1 mL) at 40° C. The resulting clear solution was stirred for about 4 h at 40° C. and subsequently cooled to 5° C. The mixture was kept at 5° C. overnight and then MTBE (1.5 v/v) was added to the mixture at room temperature leading to precipitation. The precipitate was filtered and the filter cake was dried at 60° C. in a vacuum oven for two days to give amorphous Nilotinib citrate as characterized by the powder X-ray diffractogram depicted in FIG. 31.

1. customto obtain a mixture
2. stirringThe resulting clear solution was stirred for about 4 h at 40° C.
3. customleading to precipitation
4. filtrationThe precipitate was filtered
5. customthe filter cake was dried at 60° C. in a vacuum oven for two days