反应详情

温度

5 °C

To a 1-L round bottom flask with overhead stirrer charge with 60.12 g of 4-{4-[4-(4-Fluoro-3-trifluoromethyl-phenyl)-1-methyl-1H-imidazol-2-yl]-piperidin-1-yl}-1H-pyrazolo[3,4-d]pyrimidine (prepared according to either of the above preparations without the final salt formation step), followed by 250 mL of 5% aq. MeOH. Stir the resulting slurry and add p-toluenesulfonic acid monohydrate (26.88 g) followed by a rinse forward with the remaining 50 mL of 5% aq. MeOH. Stir the resulting slurry and cool the crystals to 5° C. After 1 h at 5° C., stop stirring and filter the slurry on a Buchner funnel Rinse the flask out with 75 mL of cold 5% aq. MeOH and use this rinse to wash the filter cake. Transfer the solids to a weighing dish and dry at 50° C. in vacuo all day and all night, with a slow air bleed. The final weight is 71.44 g.

1. customprepared
2. washa rinse forward with the remaining 50 mL of 5% aq. MeOH
3. stirringStir the resulting slurry
4. stirringstop stirring
5. filtrationfilter the slurry on a Buchner funnel
6. washRinse the flask out with 75 mL of cold 5% aq. MeOH
7. washthis rinse
8. washto wash the filter cake
9. customdry at 50° C. in vacuo all day and all night, with a slow air