反应详情

Benzyl-(2,6-dichloro-3-nitro-pyridin-4-yl)-carbamic acid ethyl ester (500 mg) was dissolved in THF (3 ml) in a ReactiVial. Ammonia (7M in MeOH, 1 ml) was added, the vial was sealed, and the reaction left to stir at RT for 48 h. The reaction mixture was then pre-absorbed directly onto silica and columned on Isco Companion on a silica column (40 g, Redisep), eluting with EtOAc:heptane, increasing the gradient linearly from 10:90 to 40:60 over 10 column volumes. The desired fractions were combined and evaporated to provide the title compound as a yellow gum which solidified on scratching (305 mg)

1. customthe vial was sealed
2. waitthe reaction left
3. customThe reaction mixture was then pre-absorbed directly onto silica
4. washeluting with EtOAc
5. temperatureheptane, increasing the gradient linearly from 10:90 to 40:60 over 10 column volumes
6. customevaporated