反应详情

50 mg palladium/charcoal (10%) were added to 390 mg (0.7 mmol) 1-{1-[6-(4-benzyloxy-3,5-dimethyl-benzoyl)-pyrimidin-4-yl]-piperidin-4-yl}-1,3-dihydro-imidazo[4,5-b]pyridin-2-one in 50 mL MeOH and the mixture was hydrogenated for 40 min in a 5 psi hydrogen atmosphere at RT. The catalyst was removed by suction filtering and the filtrate was evaporated down. The residue was triturated with some MeOH, suction filtered and washed with diethyl ether. The suction filtered catalyst was decocted with 120 mL MeOH for 1 h, filtered hot and the filtrate was evaporated down. The residue was triturated with a little MeOH, suction filtered and dried. The two batches of solid were combined and purified by preparative HPLC-MS. The fractions containing the product were combined and freeze-dried.

1. customThe catalyst was removed by suction
2. filtrationfiltering
3. customthe filtrate was evaporated down
4. customThe residue was triturated with some MeOH, suction
5. filtrationfiltered
6. washwashed with diethyl ether
7. filtrationThe suction filtered catalyst
8. filtrationfiltered hot
9. customthe filtrate was evaporated down
10. customThe residue was triturated with a little MeOH, suction
11. filtrationfiltered
12. customdried
13. custompurified by preparative HPLC-MS
14. additionThe fractions containing the product
15. customfreeze-dried