反应详情

温度

105 °C

To a solution of intermediate (4) in acetic acid (45 mL) hydrogen bromide (48% solution, 15 mL) was added. The mixture was heated at 105° C. for 18 h. The reaction mixture was concentrated, then dissolved in dichloromethane (100 mL) and washed with ammonium chloride solution (100 mL). The organic layer was separated, dried over magnesium sulphate and concentrated to afford intermediate (5) as a solid. Yield: 0.65 g, 62%.

1. concentrationThe reaction mixture was concentrated
2. dissolutiondissolved in dichloromethane (100 mL)
3. washwashed with ammonium chloride solution (100 mL)
4. customThe organic layer was separated
5. dry with materialdried over magnesium sulphate
6. concentrationconcentrated