反応 #159088

反応方程式

4,4′-dibromo-2,2′-dinitro-biphenyl

sodium methoxide

Methanol

→

4,4′-dibromo-2-methoxy-2′-nitro-biphenyl

溶媒

DMF

反応条件

後処理

1. 1
   抽出The mixture was extracted with EtOAc (2×)
2. 2
   洗浄The combined organic phase was washed with water and brine
3. 3
   乾燥dried with Na2SO4
4. 4
   濃縮Concentration under reduced pressure
5. 5
   その他gave pale solid
6. 6
   その他The re-crystallization from CH3CN/MeOH

実験手順

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).

出典