反应详情

A solution of compound 6 (5.18 g, 0.030 mol) and N-bromosuccinimide (5.34 g, 0.030 mol) in chloroform (80 ml) and glacial acetic acid (80 ml) was gently heated under reflux (with stirring) for 0.5 h (glc analysis revealed a complete reaction). The reaction mixture was diluted with water and washed with dichloromethane (2×100 ml); the combined organic extracts were washed successively with water (300 ml) and aqueous potassium hydroxide (5%, 300 ml) before being dried (MgSO4). The solvent was removed in vacuo and the residue was distilled to give a colourless liquid.

1. temperatureunder reflux
2. customa complete reaction)
3. washwashed with dichloromethane (2×100 ml)
4. washthe combined organic extracts were washed successively with water (300 ml) and aqueous potassium hydroxide (5%, 300 ml)
5. dry with materialbefore being dried (MgSO4)
6. customThe solvent was removed in vacuo
7. distillationthe residue was distilled
8. customto give a colourless liquid