化学合成;制药。
化学合成; 制药
合成路线 1(1. 合成:5416-80-8)
产率:95%
合成条件:Stage #1: at 1 - 5℃; for 0.33 h; Stage #2: at 35℃; for 0.67 h; Stage #3: at 95℃; for 0.50 h; Cooling with ice
实验步骤:通用程序:将POCl 3(1.73mL,18.6mmol)缓慢滴加到搅拌和冰冷却的DMF(5.0mL)中。 将反应混合物在1-5℃下搅拌20分钟,然后缓慢加入相应的取代的2-甲基吲哚6(15.5mmol)的DMF(5.0mL)溶液。 将所得反应混合物缓慢升温至35℃并在该温度下保持40分钟。 然后将其冷却至室温。 向该混合物中加入冰(~10g),然后加入5M NaOH溶液(31mL,155mmol)。 将反应混合物在95℃加热30分钟,然后使其冷却至室温。 向该混合物中再次加入冰(~10g),并将所得反应混合物搅拌30分钟。 过滤收集所需产物并用水洗涤数次。
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