作为有机合成中间体或目标产物用于医药、农药领域,具体用途需结合应用场景进一步开发。
医药; 农药
合成路线 1(1. 合成:125849-94-7)
产率:72%
合成条件:Stage #1: at 0 - 95℃; Stage #2: With triethylamine hydrochloride In toluene at 100℃;
实验步骤:在氮气下,在3颈圆底烧瓶中,向0℃的草酰氯(179g,1.41mol)的甲苯(303mL)溶液中加入DL-乳腈(25.0g,352mmol)的溶液。在20分钟内滴加甲苯(118mL)。将反应在0℃下搅拌50分钟,然后置于70℃的油浴中,将其温热至约95℃。非常小心地加入三乙胺盐酸盐(16.8g,176mmol),因为反应易于放热。添加后,将反应在100℃下搅拌18小时。然后通过旋转蒸发在60℃水浴中除去溶剂。二乙醚(约2L)用于从粗固体中提取所需产物和污染物。另外的二乙醚(2L)用于从固体中提取几乎纯的所需产物。通过旋转蒸发将两种溶液分别浓缩至干燥。将污染的产物冷却至0℃直至形成黄色固体,通过倾析暗红色油将其分离。将该黄色固体与从第二次醚萃取得到的黄色固体(45.5g,253mmol,72%)合并。 1H NMR(400MHz,DMSOd6)δppm2.30(s,3H)。
参考文献:
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