反应详情

Iron powder (0.854 g, 15.3 mmol) is added portionwise to a mixture of 7-fluoro-1-isopropyl-5-nitro-1,3-dihydro-indol-2-one (17, 0.91 g, 3.82 mmol) and ammonium chloride (2.04 g, 38.2 mmol) in ethanol (50 ml) and water (25 ml) at 90° C. The reaction is stirred vigorously and heated for 30 min, cooled to room temperature and diluted with dichloromethane (150 mL). The mixture is filtered through celite, the organic layer separated and washed with water and brine, dried over sodium sulfate and evaporated to give the title compound as a solid. HPLC r.t. 2.97 min; MS for C11H13FN2O m/z 209.1 (M+H)+.

1. temperatureheated for 30 min
2. filtrationThe mixture is filtered through celite
3. customthe organic layer separated
4. washwashed with water and brine
5. dry with materialdried over sodium sulfate
6. customevaporated