反应详情

Sodium hydride (9 mg) was dissolved carefully in methanol (0.5 ml) and this solution then added to a solution of (2-amino-6-bromo-3-nitro-pyridin-4-yl)-benzyl-carbamic acid ethyl ester (50 mg) in THF (0.5 ml) at room temperature. The reaction was stirred under nitrogen for 2 hours then the solution pre-absorbed directly onto silica gel. The mixture was purified by chromatography on an Isco Companion, eluting with ethyl acetate:heptane, increasing the gradient linearly from 20:80 to 60:40 over several column volumes. The desired fractions were combined and evaporated to provide the title compound (23 mg) as a yellow gum.

1. customthe solution pre-absorbed directly onto silica gel
2. customThe mixture was purified by chromatography on an Isco Companion
3. washeluting with ethyl acetate
4. temperatureheptane, increasing the gradient linearly from 20:80 to 60:40 over several column volumes
5. customevaporated