3-(苄基氨基)丙酸乙酯主要用于医药和农药领域,作为中间体或活性成分。
医药; 农药
合成路线 1(1. 合成:23583-21-3)
产率:80%
合成条件:With aluminum oxide In neat (no solvent) at 95℃; for 3 h; Green chemistry
实验步骤:通用方法:在酸性氧化铝(1g,200mol%)存在下,在搅拌下回流摩尔比为1.5:1的胺(7.5mmol)和迈克尔受体(5mmol)。 使用油浴进行加热,然后通过TLC和GC进行反应直至完成。 然后使反应冷却至室温并通过滤纸过滤。 用乙酸乙酯/己烷冲洗催化剂,然后通过旋转蒸发浓缩。 使用二氧化硅填充的色谱柱纯化粗反应混合物,使用己烷/乙酸乙酯作为洗脱液。 通常,对于脂族胺,使用7:3,6:4或5:5己烷/乙酸乙酯洗脱单加合物,而对于芳族化合物,使用的溶剂混合物是8:2己烷/乙酸乙酯。 记录纯化产物的产率,然后进行IR和NMR光谱和MS光谱测定。
参考文献:
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合成路线 2(2. 合成:23583-21-3)
产率:90%
合成条件:With aluminium incorporated mesoporous aluminosilicate nano-cage material In neat (no solvent) at 20℃; for 1.50 h;
实验步骤:一般步骤:在剧烈搅拌条件下,在带有水冷凝器的双颈圆底烧瓶中进行催化液相反应。 催化剂在烘箱中在393K下预活化,随后用于反应。 在典型的方法中,将哌啶(5mmol)和丙烯酸乙酯(5mmol)的混合物加入到预活化的催化剂(25mg)中。 将反应混合物在室温下搅拌20分钟。 通过薄层色谱(TLC)监测反应进程。 反应完成后,通过离心分离催化剂。 浓缩滤液,用硅胶(100-200目),石油醚:乙酸乙酯(3:1)柱色谱纯化相应产物,通过1H NMR确认所需产物3-哌啶-1-基 - 丙酸乙酯。 并与报道的文献进行比较[15]
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