反应详情

A mixture of 1-{4-[(4,6-dimethyl-3-nitro-2-pyridinyl)amino]phenyl}-2-propanol (step 2, 500 mg, 1.66 mmol), iron powder (440 mg, 7.88 mmol), ammonium chloride (80 mg, 1.5 mmol) in ethanol/water (v/v, 31:8, 39 mL) was heated at reflux temperature for 2 h. The mixture was cooled and filtered through a pad of Celite. The filtrate was concentrated. The residue was diluted with dichloromethane (200 mL) and washed with water (2×100 mL). The organic layer was dried (MgSO4), and concentrated. Removal of solvent gave 450 mg (quant.) of the title compound as brown solids: TLC Rf 0.10 (hexane/ethyl acetate=1:1).

1. temperaturewas heated
2. temperatureat reflux temperature for 2 h
3. temperatureThe mixture was cooled
4. filtrationfiltered through a pad of Celite
5. concentrationThe filtrate was concentrated
6. additionThe residue was diluted with dichloromethane (200 mL)
7. washwashed with water (2×100 mL)
8. dry with materialThe organic layer was dried (MgSO4)
9. concentrationconcentrated
10. customRemoval of solvent