反应详情

To a stirred suspension of nitro compound 417 (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 was heated to reflux for 2 hrs, cooled to room temperature and filtered through celite. The filtrate was concentrated, diluted with minimal amount of methanol and treated with AcOEt/hexanes, to afford title compound 418 (463 mg, quantitative yield, ammonium salt) as a yellow solid. LCMS: 340.0 (M+H)+.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 2 hrs
3. filtrationfiltered through celite
4. concentrationThe filtrate was concentrated
5. additiondiluted with minimal amount of methanol
6. additiontreated with AcOEt/hexanes