反应详情

温度

0 °C

Ethanesulfonyl chloride (4.5 mL, 47.4 mmol) was added dropwise to a solution of 5-bromo-3-(4-piperidinyl)-1H-indole-7-carboxamide hydrochloride (8.49 g, 23.7 mmol) and triethylamine (13.2 mL, 94.7 mmol) in DMF (80 mL) at 0° C. (bath temperature). The reaction mixture was stirred at 0° C. for 45 min. and was then poured into a 2:1 mixture of EtOAc/H2O (300 mL). The resulting precipitate was filtered off, washed with EtOAc (2×50 mL), and set aside. The EtOAc/H2O bilayer was separated, and the aqueous layer was extracted with EtOAc (2×100 mL). The combined organic layers were washed with saturated NaCl (1×100 mL), dried (MgSO4), filtered, and concentrated under reduced pressure. The crude product was combined with the precipitate isolated above and washed with MeOH (1×10 mL) to give 8.19 g of the title compound (83%).

1. filtrationThe resulting precipitate was filtered off
2. washwashed with EtOAc (2×50 mL)
3. customThe EtOAc/H2O bilayer was separated
4. extractionthe aqueous layer was extracted with EtOAc (2×100 mL)
5. washThe combined organic layers were washed with saturated NaCl (1×100 mL)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customisolated above and
10. washwashed with MeOH (1×10 mL)