Table 3.
Entry | Purification method | Fe impurity in 15 (ppm) |
1 | Extractiona + column chromatographyb | 54 |
2 | Extractiona | 1097 |
3 | Extractiona + recrystallizationc | 300 |
aWashing subsequently with sat. aq NaHCO3 and brine, extraction with dichloromethane. bSilica flash cartridge applying a heptane/ethyl acetate gradient. cRecrystallization from a 2 M HCl solution.