反应详情

温度

0 °C

A suspension of NaH (600 mg, 15 mmol, 60% in mineral oil) in DMF (10 mL) at 0° C. is treated with 5-fluoro-3-(2-pyridin-3-yl-ethyl)-1H-indole (240 mg, 1 mmol) and stirred at 0° C. for 0.5 h. The mixture is treated with HOSA (565 mg, 5 mmol) portion wise and warmed to rt over 2 h. The mixture is then poured over ice, filtered through a pad of Celite, and extracted with EtOAc (3×1050 mL). The combined organic layer is dried (Na2SO4), filtered and concentrated in vacuo to afford 5-fluoro-3-(2-pyridin-3-yl-ethyl)-indol-1-ylamine, which is used in the next step without further purification.

1. additionThe mixture is treated with HOSA (565 mg, 5 mmol) portion wise
2. temperaturewarmed to rt over 2 h
3. additionThe mixture is then poured over ice
4. filtrationfiltered through a pad of Celite
5. extractionextracted with EtOAc (3×1050 mL)
6. dry with materialThe combined organic layer is dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo