反应详情

温度

35 °C

To a stirred suspension of Vemurafenib base (1.5 g, 3.1 mmol) and 15 ml acetone (T=30-35° C.), 0.9 ml (3.1 mmol) choline (45% in methanol) was added. The obtained solution was stirred for 5 min at 35° C. then cooled to 5° C., stirred at this temperature for 30 min and then allowed to warm to RT. During overnightstirring in the open vial, the solvent evaporated. To the oily residue, 5 ml ethanol was added. The mixture was placed in an ultrasonic bath until a clear solution was obtained. After the solution was stored in the refrigerator for 3 days, a precipitate was formed which was filtered off, washed with 2 ml ethanol and dried at RT O/N. 0.54 g (yield: 29.7%) Vemurafenib choline salt was isolated in high purity (HPLC/UV: 99.4 area %).

1. additionwas added
2. temperaturethen cooled to 5° C.
3. stirringstirred at this temperature for 30 min
4. temperatureto warm to RT
5. customthe solvent evaporated
6. additionTo the oily residue, 5 ml ethanol was added
7. customThe mixture was placed in an ultrasonic bath until a clear solution
8. customwas obtained
9. waitAfter the solution was stored in the refrigerator for 3 days
10. customa precipitate was formed which
11. filtrationwas filtered off
12. washwashed with 2 ml ethanol
13. customdried at RT O/N