反应详情

To a suspension of 3-(3-nitropyridin-2-yl)aniline (400 mg), N,N′-bis(tert-butoxycarbonyl)thiourea (616 mg) and diisopropylethylamine (0.745 ml) in dichloromethane (18.6 ml) was added 1-methyl-2-chloropyridinium iodide (618 mg), and the mixture was stirred for 16 hours. The mixture was diluted with ethyl acetate, washed with water and brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 30 g, n-hexane:ethyl acetate=4:1) to give N,N′-bis(tert-butoxycarbonyl)-N″-(3-(3-nitropyridin-2-yl)phenyl)guanidine (730 mg).

1. washwashed with water and brine
2. dry with materialdried over magnesium sulfate
3. customevaporated under reduced pressure
4. customThe residue was purified by column chromatography (silica gel 30 g, n-hexane:ethyl acetate=4:1)