反应详情

Iron powder (0.77 g, 0.0138 mol) is added in small portions to a mixture of 4-fluoro-3-methyl-6-nitro-1,3-benzoxazol-2(3H)-one (Step 6, 0.73 g, 3.44 mmol) and ammonium chloride (1.84 g, 3.44 mmol) in ethanol (30 ml) and water (15 ml) at 95° C. The reaction mixture is stirred vigorously and heated for 1 h, cooled to room temperature, and diluted with dichloromethane (150 ml). The mixture is filtered, washed with water and saline, dried (MgSO4) and evaporated to give product as a tan solid suitable for use in the next step (0.64 g, 99%).

1. temperatureheated for 1 h
2. filtrationThe mixture is filtered
3. washwashed with water and saline
4. dry with materialdried (MgSO4)
5. customevaporated
6. customto give product as a tan solid suitable for use in the next step (0.64 g, 99%)