反应详情

7-Fluoro-5-nitro-2,3-dihydro-1,4-benzodioxin (6.96 g, 35 mmol) and 5% Pd/C (4 g) in MeOH (500 ml) was stirred overnight in the presence of hydrogen at atmospheric pressure at rt. The catalyst was filtered off and solvent removed; the residue was dissolved in MeOH (100 ml), more 5% Pd/C (paste, 3 g) was added and mixture stirred overnight in presence of hydrogen (45 psi) at rt. The catalyst was filtered off and solvent removed; the residue treated with DCM (20 ml), the solid filtered off and compound in DCM loaded on silica (pre-wet with petroleum ether) and purified using a 10%-50% EtOAc: 40-60 petroleum ether gradient to provide the desired compound (3 g, 51%).

1. filtrationThe catalyst was filtered off
2. customsolvent removed
3. dissolutionthe residue was dissolved in MeOH (100 ml)
4. additionmore 5% Pd/C (paste, 3 g) was added
5. filtrationThe catalyst was filtered off
6. customsolvent removed
7. additionthe residue treated with DCM (20 ml)
8. filtrationthe solid filtered off
9. custompurified