氯化亚铜实验中做为催化剂需要注意哪些?
来自:上海荣建化工厂
42人民币
发布时间:2012-10-30
关注次数:563
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今天想做一个将苯环上的碘经过化合反应变成甲氧基。实验过程是将氯化亚铜做为催化剂的,可是我做了好几次都没有做成功。参考资料上业没有讲什么需要注意的地方,所以想请教下在做这种用氯化亚铜做催化剂反应的时候,在哪些地方需要特别注意的?
参考资料:Compound 2 (500 mg, 1.0 mmol), NaOMe (290 mg, 5.4 mmol), and CuCl (27 mg, 0.27 mmol) were suspended in a mixture of MeOH (5mL) and DMF (3 mL) and heated at 80 °C. After 16 h, the suspension
was slowly cooled down and a mixture of diisopropyl ether (7mL), H2O (15 mL), and 5% aq NH4Cl solution (10 mL) were added and the resulting solution was stirred at r.t. After 5 h, the solution was filtered over Celite and the filtrate was extracted with CH2Cl2(4 ×). The combined organic layers were washed with aq 5 N NaOH and dried (Na2SO4). Concentration in vacuo gave 309 mg (99%) of 3 as a brown solid;
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