关于钯催化的格氏试剂反应？最近一直在做这个反应，文献没有注明反应具体温度，文献用的是ni(dppp)cl2，0.01当量。做的时候用的是thf，pd(dppf)cl2 0.02当量，70度12小时， 无水 无氧操作的，反应产率为0，原料没有反应。求助各位朋友这是什么原因？或者希望各位能给达到这个合成目的的其他路径…… 以下是文献原文，6a就是图中的b a solution of 6a (3.78 g, 13.0 mmol) was dissolved in dry thf (15 ml) and purged with argon. at room temperature, memgbr (4.33 ml, 13.0mmol, 3.0 m in diethyl ether) was added dropwise. then the reaction mixture was gently refluxed for 1 h before being transferred via cannula to a cooled solution (0 °c) of 6a (3.78 g, 13.0 mmol) and ni(dppp)cl2 (700 mg, 0.130 mmol) in dry thf (15 ml). after refluxing for one night, the reaction mixture was allowed to cool to room temperature and poured into a 0.5 m hcl solution. the green precipitate was filtered off, which was a first fraction of the pure product. then the aqueous layer was extracted twice with diethyl ether, and the organic extracts were washed with a nahco3 solution and brine. after drying over mgso4, the solvent was removed by rotary evaporation. 查看更多1个回答 . 16人已关注
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