反应详情

A solution of 2-(5-bromo-2-(2-chloroethyl)pyridin-3-yl)-4-fluoro-1H-indole (800 mg, 2.26 mmol) and cesium carbonate (1.47 g, 4.52 mmol) in 25 mL of DMF was heated at 80° C. for 1 hour. The mixture was concentrated in vacuo to remove DMF, and then the residue was suspended in water and EA. After extraction with EA, the combined organic phase was washed with brine, dried over sodium sulfate and concentrated to afford crude 2-bromo-11-fluoro-5,6-dihydroindolo[2,1-f][1,6]naphthyridine (600 mg, yield: 83.6%) which was used directly in the next step without further purification. 1H-NMR (CDCl3, 400 MHz) δ 8.48 (s, 1H), 8.11 (s, 1H), 7.11˜7.17 (m, 2H), 6.97 (s, 1H), 6.78˜6.82 (m, 1H), 4.34˜4.37 (m, 2H), 3.34˜3.37 (m, 2H). MS (M+H)+: 317/319.

1. concentrationThe mixture was concentrated in vacuo
2. customto remove DMF
3. extractionAfter extraction with EA
4. washthe combined organic phase was washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated