作为有机合成中间体,用于构建复杂有机分子结构,其卤代基团可参与偶联反应等后续化学转化。
有机合成中间体
合成路线 1(1. 合成:19821-80-8)
产率:91%
合成条件:Stage #1: With n-butyllithium; diisopropylamine In tetrahydrofuran; hexanes at -75℃; for 2 h; Stage #2: With iodine In tetrahydrofuran; hexanes
实验步骤:实施例1:1,3-二溴-2-碘苯(II); 将二异丙胺(0.14L,0.10kg,1.0mol)和1,3-二溴苯(0.12L,0.24kg,1.0mol)连续加入到正丁基锂(1.0mol)的四氢呋喃(2.0L)和己烷(一起)溶液中( 在-75℃下0.64L)。 在-75℃下2小时后,加入碘(0.26kg,1.0mol)的四氢呋喃(0.5L)溶液。 蒸发溶剂,将残余物溶于乙醚(1.0L)中。 用10%硫代硫酸钠水溶液(2×0.1L)洗涤后,有机层用硫酸钠干燥,然后蒸发至干。 从乙醇(1.0L)中结晶后,得到0.33kg(91%)无色小片; m.p.205℃。 99℃,100℃; 1H-NMR(CHCl3,400MHz):δ= 7.55(d,J = 8.1Hz,2H),7.07(t,J-8.1Hz,2H); C6H3Br2I(361.80):计算值( 百分比)C 19.92,H 0.84; 实测值C 19.97,H 0.80。
参考文献:
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