反应详情

A mixture of methyl 5-nitro-(pyrid-2-yl)-thioacetate (6.3 g, Reference Example 2) iron powder (12 g), ammonium chloride (1 g), ethanol (150 ml) and water (150 ml) was heated at reflux for 2 hours. The reaction mixture was cooled and then filtered through a pad of diatomaceous earth. The filtrate was evaporated and the residue was subjected to flash chromatography on silica gel eluting with a mixture of ethyl acetate and pentane (1:1, v/v) to give the title compound as a yellow oil (3.0 g).

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. temperatureThe reaction mixture was cooled
4. filtrationfiltered through a pad of diatomaceous earth
5. customThe filtrate was evaporated
6. additionthe residue was subjected to flash chromatography on silica gel eluting with a mixture of ethyl acetate and pentane (1:1