反应详情

A mixture of 6-chloro-3-nitro-2-(pyridine-2-carbonyl)indole (step 3, 92 mg, 0.30 mmol), ammonium chloride (8 mg, 0.15 mmol) and iron powder (89 mg, 1.52 mmol) in 70% aqueous ethanol (6 ml) was heated at reflux for 2 h, and then cooled and filtered through a pad of Celite. The pad was washed copiously with a mixture of ethanol/ethyl acetate (1:1 v/v) and the combined washing evaporated. The residue was diluted with ethyl acetate (50 ml), washed with saturated aqueous sodim bicarbonate (30 ml) and dried (Na2SO4). Removal of solvent gave product as crystals.

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. temperaturecooled
4. filtrationfiltered through a pad of Celite
5. washThe pad was washed copiously with a mixture of ethanol/ethyl acetate (1:1 v/v)
6. washthe combined washing
7. customevaporated
8. additionThe residue was diluted with ethyl acetate (50 ml)
9. washwashed with saturated aqueous sodim bicarbonate (30 ml)
10. dry with materialdried (Na2SO4)
11. customRemoval of solvent
12. customgave product as crystals