反应详情

温度

100 °C

A mixture containing methyl 1-chloro-5H-pyrido[4,3-b]indole-4-carboxylate and LiNH2 (prepared in situ from ammonia and n-BuLi; 1.0 M in THF; 3.5 equiv) in THF (0.09 M) was heated in a microwave reactor at 100° C. for 1 min in a sealed tube. The reaction mixture was cooled to room temperature and partitioned between EtOAc and saturated NaHCO3. After separation of the organic phase, the aqueous phase was extracted again with EtOAc, and the combined organic phases were washed with brine, dried over MgSO4 and filtered. After evaporation of the organic solvent, the residue was purified by flash chromatography (10-70% EtOAc in hexanes) to provide the title compound as a white solid.

1. temperatureThe reaction mixture was cooled to room temperature
2. custompartitioned between EtOAc and saturated NaHCO3
3. customAfter separation of the organic phase
4. extractionthe aqueous phase was extracted again with EtOAc
5. washthe combined organic phases were washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customAfter evaporation of the organic solvent
9. customthe residue was purified by flash chromatography (10-70% EtOAc in hexanes)