反应详情

温度

75 °C

The product from Step 3 (7.42 g, 25.2 mmol) in acetic acid (80 mL) was treated with iron powder (5.65 g, 100.95 mmol) portionwise over 1 h while the temperature was maintained between 70-80° C. The hot reaction mixture was quickly filtered through a pad of celite and washed with methanol. The combined filtrates concentrated to give a dark red residue was treated with NaHCO3 and extracted with ethyl acetate. The organic layers were washed brine, dried over Na2SO4 and concentrated to afford the title compound (6.1 g, 95%). MS (ES+) m/e 264/266 [M+H]+.

1. filtrationThe hot reaction mixture was quickly filtered through a pad of celite
2. washwashed with methanol
3. concentrationThe combined filtrates concentrated
4. customto give a dark red residue
5. extractionextracted with ethyl acetate
6. washThe organic layers were washed brine
7. dry with materialdried over Na2SO4
8. concentrationconcentrated