反应详情

To a stirred suspension of nitro compound 338 (370 mg, 1.00 mmol) in a mixture of MeOH (20 mL) and water (10 mL) were added iron powder (280 mg, 5.01 mmol) and NH4Cl (107 mg, 2.00 mmol). The reaction mixture heated to reflux for 2 hrs, cooled down to room temperature, filtered through Celite, and rinsed with methanol. The filtrate was concentrated, diluted a bit with methanol, precipitated with AcOEt/hexanes to afford title compound 339 (463 mg, quantitative yield, ammonium salt) as a yellow solid. MS (m/z): 340.0 (M+H)+.

1. temperatureThe reaction mixture heated
2. temperatureto reflux for 2 hrs
3. filtrationfiltered through Celite
4. washrinsed with methanol
5. concentrationThe filtrate was concentrated
6. additiondiluted a bit with methanol
7. customprecipitated with AcOEt/hexanes