反应详情

温度

15 °C

The product of step (a) (88 g, 0.5 m) in acetic acid (1 l) was treated with bromine (26 ml, 0.5 m) over 15 minutes, maintaining an internal temperature of ca, 15° C. The mixture was allowed to warm to room temperature overnight. The solvent was evaporated off under reduced pressure and the residue partitioned between water and diisopropyl ether. The organic phase was dried (MgSO4) and evaporated to give a residue which on recrystallising from hexane gave the title compound as white needles, mp 68-70.

1. temperatureto warm to room temperature overnight
2. customThe solvent was evaporated off under reduced pressure
3. customthe residue partitioned between water and diisopropyl ether
4. dry with materialThe organic phase was dried (MgSO4)
5. customevaporated
6. customto give a residue which
7. customon recrystallising from hexane