反应详情

温度

50 °C

To a solution of 1-tert-butoxycarbonyl-4-methyl-5-nitrobenzimidazole (8 g) in methanol (40 mL)/ethyl acetate (400 mL)is added palladium-on-carbon (Pd/C) (10%, 0.5 g) and ammonium formate (7.27g). The mixture is stirred at 50° C. for 2 hours, then filtered on Celite, with methanol wash of the solids. The filtrate is rotary evaporated and the residue partitioned between water and ethyl acetate. The organic layer is washed with saturated ammonium chloride, dried over magnesium sulfate, filtered and rotary evaporated to afford pure 5-amino-1-tert-butoxycarbonyl-4-methylbenzimidazole as an off-white solid.

1. filtrationfiltered on Celite, with methanol
2. washwash of the solids
3. customThe filtrate is rotary evaporated
4. customthe residue partitioned between water and ethyl acetate
5. washThe organic layer is washed with saturated ammonium chloride
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customrotary evaporated