反应详情

温度

55 °C

Bromine (20.5 mL, 0.4 mol) was added to a solution of KOH (72.9 g, 1.3 mol) in water (250 mL) at 0° C. To the resulting solution was slowly added compound 2 (16.0 g, 0.1 mol) at 0° C. The reaction mixture was heated at 55° C. overnight and quenched with Na2S2O3 (14.8 g, 0.094 mol). The mixture was acidified to pH 2-3 with conc. HCl (40˜50 mL). The precipitate was collected by filtration, and washed with water. The crude product 3 was dried under high vacuum and used without further purification (15.4 g, 0.095 mol, 95%).

1. customat 0° C
2. filtrationThe precipitate was collected by filtration
3. washwashed with water
4. dry with materialThe crude product 3 was dried under high vacuum
5. customused without further purification (15.4 g, 0.095 mol, 95%)