反应详情

温度

0 °C

To a stirred solution of tert-butyl 2-[4-(4-chloro-2-ethyl-6-methyl-1H-imidazo[4,5-c]pyridin-1-yl)phenyl]ethylcarbamate (step 3, 90 mg, 0.22 mmol) in dichloromethane (8.5 ml) was added trifluoroacetic acid (1.0 ml, 13.0 mmol) at 0° C., and the mixture was stirred at 0° C. for 30 min, then at room temperature for 5 h. The mixture was concentrated, and diluted with dichloromethane (50 ml), washed with saturated aqueous NaHCO3 solution (10 ml) and brine (10 ml). The organic layer was dried (MgSO4), and concentrated. Purification by PTLC eluting with ethyl acetate to afford 50 mg (73%) of the title compound as a brown oil.

1. waitat room temperature for 5 h
2. concentrationThe mixture was concentrated
3. additiondiluted with dichloromethane (50 ml)
4. washwashed with saturated aqueous NaHCO3 solution (10 ml) and brine (10 ml)
5. dry with materialThe organic layer was dried (MgSO4)
6. concentrationconcentrated
7. customPurification by PTLC
8. washeluting with ethyl acetate