反应详情

A mixture of 18.9 g (0.082 mol) 3-nitro-2,4-bis(methylthio)-6-methylpyridine and 18.9 g Raney nickel in 600 ml. 1,4-dioxane and 300 ml methanol was shaken with hydrogen (15 psi) in a Parr hydrogenation apparatus for 3.5 hours. The catalyst was filtered and the filtrate was concentrated to dryness in vacuo. The solid residue was chromatographed on silica gel (650 g), eluting with 9:1 hexane/ethyl acetate to yield 14.0 g. (85% yield) of the title compound as an off white solid.

1. filtrationThe catalyst was filtered
2. concentrationthe filtrate was concentrated to dryness in vacuo
3. customThe solid residue was chromatographed on silica gel (650 g)
4. washeluting with 9:1 hexane/ethyl acetate
5. customto yield 14.0 g