2-氟-5-溴硝基苯的合成
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Synthesis of 2-fluoro-5-bromonitrobenzene
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    摘要:

    采用冰醋酸作为溶剂,以邻氟硝基苯为原料, N-溴代丁二酰亚胺(NBS)为溴代试剂,合成了2-氟-5-溴硝基苯。所得目标产物通过GC-MS定性、GC定量检测。结果表明,最佳反应条件为邻氟硝基苯:NBS(摩尔比)=1:1.05,以冰醋酸作溶剂,温度10 ℃,反应2 h,在此条件下2-氟-5-溴硝基苯的收率为98.6%,原料转化率100%。该反应条件温和,易于控制,重复性好。

    Abstract:

    2-fluoro-5-bromonitrobenzene was prepared from 2-fluoronitrobenzene using the solvent acetic acid (CH3COOH) instead of sulfuric acid or 2-fluoro-5-bromonitrobenzene was prepared from 2-fluoronitrobenzene using the solvent acetic acid (CH3COOH) instead of sulfuric acid or boron trifluoride, using N-bromosuccinimide (NBS) as bromide reagent. The reaction condition was mild and easy to be controlled, the target product qualitative was analysised by GC-MS and quantification was analysised by GC. The best yield(98.6%) of 2-fluoro-5-bromonitrobenzene and conversion (100%) of 2-fluoronitrobenzene were obtained under optimized conditions that n(2-fluoronitrobenzene):n(NBS) =1:1.05, the reaction temperature was 10 ℃ and the reaction time was 2 h. The repeat experiments showed that the technology had a good repeatability under above optimum conditions.

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陈兴权.2-氟-5-溴硝基苯的合成[J].精细化工,2012,29(1):

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  • 收稿日期:2011-09-20
  • 最后修改日期:2011-11-08
  • 录用日期:2011-11-11
  • 在线发布日期: 2011-12-26
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