今天想做一個將苯環(huán)上的碘經過化合反應變成甲氧基。實驗過程是將氯化亞銅做為催化劑的,可是我做了好幾次都沒有做成功。參考資料上業(yè)沒有講什么需要注意的地方,所以想請教下在做這種用氯化亞銅做催化劑反應的時候,在哪些地方需要特別注意的?
參考資料: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;