关于乌尔曼反应？求助大家，最近在做这个反应，文献没有给出具体温度而且文献用的是ni(dppp)cl2。因为实验室暂时没有，我做的时候用的pd(dppf)cl2，按文献thf溶剂，70度10小时， 无水 无氧操作的。结果产率为0，原料没有反应……求助应该怎么改进实验操作呀？ 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13个回答 . 19人已关注
第1天
关注盖德视界
添加小助手
