HRID79851
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
The mixture of 1,4-dibromo-2-nitro-benzene (25 g, 89 mmol) and copper powder (12.5 g, 197 mmol) in DMF (150 ml) was heated at 137 C for 2 hours. The mixture was cooled to 25° C. and was quenched with water. The mixture was extracted with EtOAc (2×). The combined organic solution was washed with water and brine and was dried with Na2SO4. Concentration and purification by flash column chromatography (hexanes/EtOAc) gave 4,4′-dibromo-2,2′-dinitro-biphenyl (13.6 g).
WORKUP
后处理
- temperaturewas heated at 137 C for 2 hours
- customwas quenched with water
- extractionThe mixture was extracted with EtOAc (2×)
- washThe combined organic solution was washed with water and brine
- dry with materialwas dried with Na2SO4
- concentrationConcentration and purification by flash column chromatography (hexanes/EtOAc)