反应详情

温度

0 °C

Into a solution of tert-butyl (2-(7-oxo-7-((pyridin-3-ylmethyl)amino)heptanamido)phenyl)carbamate (1.2 g, 2.73 mmol) in EtOAc (50 mL) were passed HCl (gas) at 0° C. The mixture was stirred for 30 min at 0° C. under HCl (gas). A white solid precipitated and was filtered. The white solid was collected and poured into a solution of 5% Na2CO3 in water (100 mL). The resulting mixture was extracted by EtOAc (100 mL×2). The organic layers were combined, dried with anhydrous Na2SO4 and concentrated under reduce pressure. The crude solid was recrystallized in EtOAc to afford the desired compound (0.6 g, yield 64.6%) as an off-white solid.

1. customat 0° C
2. customA white solid precipitated
3. filtrationwas filtered
4. customThe white solid was collected
5. additionpoured into a solution of 5% Na2CO3 in water (100 mL)
6. extractionThe resulting mixture was extracted by EtOAc (100 mL×2)
7. dry with materialdried with anhydrous Na2SO4
8. concentrationconcentrated
9. customThe crude solid was recrystallized in EtOAc