反应详情

To a solution of diethyl 2-chloro-3-methoxy-4-nitrobenzylphosphonate (Compound 54F, 1 g, 2.96 mmol) in ethanol (15 mL), and iron powder (1.63 g, 29.6 mmol) was added aqueous 2N HCl (5 mL). The reaction mixture was heated to reflux for 1.5 h. The reaction mixture was cooled to RT and saturated solution of Na2CO3 was added until the pH was 9. The reaction mixture was filtered through celite and concentrated to give the residue. It was dissolved in ethyl acetate (25 mL) and washed with water, dried over sodium sulfate, filtered and concentrated to give the required product (89%, 900 mg). 1H NMR (300 MHz, CDCl3) δ 7.01 (d, 1H), 6.62 (d, 1H), 4.00-4.19 (m, 4H), 3.83 (s, 3H), 3.25 (d, 2H), 1.23 (t, 6H).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 1.5 h
3. filtrationThe reaction mixture was filtered through celite and
4. concentrationconcentrated
5. customto give the residue
6. washwashed with water
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated