反应详情

To a solution of compound 286 (1.5 g, 7.5 mmol) in methanol (62 ml) and water (12 ml) under nitrogen at room temperature was added ammonium chloride (0.604 g, 11.3 mmol) and iron (1.68 g, 30.1 mmol). The resulting mixture was heated to reflux for 30 min then filtered through celite. The celite pad was rinsed with methanol. The filtrate and washings were combined and concentrated and the residue was purified via Biotage (linear gradient 0-20%, methanol/dichloromethane; 25M column) to afford compound 287 as a yellow solid (1.27 g, 7.51 mmol, quantitative). MS (m/z): 170.1 (M+H).

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 30 min
3. filtrationthen filtered through celite
4. washThe celite pad was rinsed with methanol
5. concentrationconcentrated
6. customthe residue was purified via Biotage (linear gradient 0-20%, methanol/dichloromethane; 25M column)