反应详情

A mixture of 4-formyl-2-methoxy-3-nitrophenyl acetate (Step 1, 438 g, 1.8 mol) and potassium carbonate (506 g, 3.7 mol) in MeOH (4000 mL) was stirred at room temperature for 16 h. The reaction mixture was concentrated under reduced pressure to afford a viscous oil. This was dissolved in water, acidified using a solution of HCl (2 N) and extracted with EtOAc. The organic layer was washed with brine, dried (MgSO4) and filtered. The solvent was concentrated under reduced pressure to ⅓ volume and the resulting solids were filtered and air-dried to give the title compound (317 g, 88%): 1H NMR (DMSO-d6) δ: 9.69 (1H, s), 7.68 (1H, d), 7.19 (1H, d), 3.82 (3H, s).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customto afford a viscous oil
3. extractionextracted with EtOAc
4. washThe organic layer was washed with brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationThe solvent was concentrated under reduced pressure
8. filtrationthe resulting solids were filtered
9. customair-dried