反应详情

A round bottom flask equipped with a stir bar was charged with N-(2-aminopyrimidin-5-yl)-2-methyl-5-nitrobenzamide 8 (300 mg, 1.1 mmol), 10% Pd/C (˜150 mg), EtOAc (24 mL) and MeOH (6 mL). The mixture was purged with H2 (3× evacuation and back-fill cycles) then allowed to stir under an H2 balloon. After 24 h, TLC and LCMS indicated that the starting material was completely consumed. The mixture was filtered through a pad of Celite, washing with MeOH and CH2Cl2. Recrystallization from MeOH/CH2Cl2 afforded 5-amino-N-(2-aminopyrimidin-5-yl)-2-methylbenzamide 9 as a pale yellow crystalline solid.

1. customA round bottom flask equipped with a stir bar
2. customThe mixture was purged with H2 (3× evacuation and back-fill cycles)
3. customwas completely consumed
4. filtrationThe mixture was filtered through a pad of Celite
5. washwashing with MeOH and CH2Cl2
6. customRecrystallization from MeOH/CH2Cl2