反应详情

温度

30 °C

Concentrated HCl (1 mL) was added to a solution of (4,5-difluoro-7-nitro-benzofuran-6-yl)-(2-fluoro-4-iodo-phenyl)-amine (0.260 g, 0.599 mmol) in THF (5 mL) at 0° C. This was followed by the addition of zinc dust (0.179 g, 5.99 mmol) at 0° C. The reaction mass was stirred for 1 hour at 20-40° C. The reaction was monitored by TLC (20% ethyl acetate in hexane). The reaction mass was concentrated under reduced pressure and the concentrate was extracted with ethyl acetate (50 mL). The organic layer was washed with water, brine solution, dried over sodium sulphate and concentrated under reduced pressure to afford 0.240 g of the crude compound which used for the next step without further purification. 1H NMR (CDCl3, 300 MHz): δ 7.53 (d, 1H), 7.49 (dd, 1H), 7.20 (d, 1H), 6.00 (d, 1H), 6.20 (t, 1H), 5.42 (bs, 1H), 4.10 (bs, 2H).

1. concentrationThe reaction mass was concentrated under reduced pressure
2. extractionthe concentrate was extracted with ethyl acetate (50 mL)
3. washThe organic layer was washed with water, brine solution
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated under reduced pressure