HRID79852

反应详情

EQUATION

反应方程式

HRID 79852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To the solution of 4,4′-dibromo-2,2′-dinitro-biphenyl (6.58 g, 16.5 mmol) in DMF (50 ml) at 0° C. was added a solution of sodium methoxide in Methanol (4.4 M, 4.5 ml, 19.8 mmol). The mixture was stirred at 25° C. for 12 hours and was poured into ice-water (140 ml). The mixture was extracted with EtOAc (2×). The combined organic phase was washed with water and brine and dried with Na2SO4. Concentration under reduced pressure gave pale solid. The re-crystallization from CH3CN/MeOH gave 4,4′-dibromo-2-methoxy-2′-nitro-biphenyl as a white solid (3.76 g).

WORKUP

后处理

  1. extractionThe mixture was extracted with EtOAc (2×)
  2. washThe combined organic phase was washed with water and brine
  3. dry with materialdried with Na2SO4
  4. concentrationConcentration under reduced pressure
  5. customgave pale solid
  6. customThe re-crystallization from CH3CN/MeOH