反应详情

温度

23 °C

To 4-bromobenzoic acid (5.00 g, 24.9 mmol, 1.00 equiv) and N-hydroxysuccinimide (3.66 g, 31.8 mmol, 1.28 equiv) in a round-bottom flask in dioxane (120 mL) was added an dioxane solution (30 mL) that contained 1,3-dicyclohexylcarbodiimide (DCC) (6.77 g, 32.8 mmol, 1.32 equiv) dropwise over 5 min at 23 ° C. The reaction mixture was stirring at 23 ° C. for 24 h. The reaction mixture was concentrated in vacuo and the crude product was obtained by recrystallization in a cold acetone. The crude product was further purified by chromatography on silica gel eluting with hexanes/EtOAc 2:1 (v/v) to afford 6.34 g of the title compound as a colorless solid (86%).

1. customdropwise over 5 min
2. customat 23 ° C
3. concentrationThe reaction mixture was concentrated in vacuo
4. customthe crude product was obtained by recrystallization in a cold acetone
5. customThe crude product was further purified by chromatography on silica gel eluting with hexanes/EtOAc 2:1 (v/v)