反应详情

Benzyl-(2,6-dibromo-3-nitro-pyridin-4-yl)-carbamic acid ethyl ester (7.50 g) was dissolved in 2-methyl-tetrahydrofuran (15 ml) and the solution placed in a sealable vessel. Concentrated aqueous ammonia solution (15 ml) was added and the vial was then sealed and the bi-phasic mixture left to stir vigorously at room temperature for 36 hours. The reaction mixture was then transferred to a separating funnel and ethyl acetate (120 ml) and water (120 ml) were added. The phases were separated, and then the organics washed with brine (100 ml), dried (MgSO4), and evaporated to a yellow oil. Upon standing, a yellow solid crystallised. This was collected by filtration and washed with pentane, providing the title compound (6.64 g) as a yellow solid.

1. customthe solution placed in a sealable vessel
2. customthe vial was then sealed
3. waitthe bi-phasic mixture left
4. customThe reaction mixture was then transferred to a separating funnel
5. customThe phases were separated
6. washthe organics washed with brine (100 ml)
7. dry with materialdried (MgSO4)
8. customevaporated to a yellow oil
9. customa yellow solid crystallised
10. filtrationThis was collected by filtration
11. washwashed with pentane