反应详情

温度

60 °C

2-Fluoro-4-methyl-5-nitrobenzoic acid (900 mg, 4.52 mmol) in MeOH (70 ml) was treated with ammonium formate 1 (425 mg, 22.60 mmol) and Pd (Carbon) (144 mg, 1.356 mmol). The mixture was degassed thoroughly refilling with nitrogen and heated to 60° C. for 2 hrs. The mixture was filtered through silica and washed with MeOH. The filtrate was passed through SCX-2 resin (30 g 0.67 mmol/g) eluting with MeOH (250 ml) followed by 2M ammonia in MeOH (250 ml). The ammonia/MeOH washings were evaporated to dryness and the resulting crude residue was purified by recrystallisation from MeOH to afford the title compound;

1. customThe mixture was degassed thoroughly
2. filtrationThe mixture was filtered through silica
3. washwashed with MeOH
4. washeluting with MeOH (250 ml)
5. customThe ammonia/MeOH washings were evaporated to dryness
6. customthe resulting crude residue was purified by recrystallisation from MeOH