反应详情

To a suspension of 1-chloro-5H-pyrido[4,3-b]indole-4-carboxamide (Example 10 Step 3) in AcOH (0.15 M) at room temperature was added Br2 (10 equiv) to provide a homogeneous mixture. After standing at room temperature a precipitate formed, and after 1 h, a suspension of Zn powder (excess) in THF was added in a cold water bath. After a period of 10 min, the reaction mixture was poured over THF/EtOAc and saturated NaHCO3. After separation of the organic phase, the aqueous phase was extracted again with THF/EtOAc, and the combined organic phases were washed with brine, dried over MgSO4 and filtered. After evaporation of the organic solvents, the residue was purified by flash chromatography (10-70% EtOAc in hexanes) to provide the title compound as a yellow solid.

1. customto provide a homogeneous mixture
2. customAfter standing at room temperature
3. customformed
4. additionwas added in a cold water bath
5. waitAfter a period of 10 min
6. customAfter separation of the organic phase
7. extractionthe aqueous phase was extracted again with THF/EtOAc
8. washthe combined organic phases were washed with brine
9. dry with materialdried over MgSO4
10. filtrationfiltered
11. customAfter evaporation of the organic solvents
12. customthe residue was purified by flash chromatography (10-70% EtOAc in hexanes)