化学合成,Wittig烯化反应试剂。
化学合成
合成路线 1(1. 合成:1779-58-4)
产率:100%
合成条件:at 20℃; for 17 h;
实验步骤:一般步骤:向搅拌的PPh 3(1.7g,6.7mmol)的乙酸乙酯溶液中,在室温下加入2-溴乙酸甲酯(0.62μL,6.5mmol)的乙酸乙酯溶液.17小时后,得到白色沉淀物。过滤收集,用乙醚洗涤三次,在空气中干燥,得到(2-甲氧基-2-氧代乙基)三苯基溴化鏻(4,2.49g),为白色固体,几乎定量收率。将溴化鏻4(2.0g,4.81mmol)加入到乙醇钠(340mg)的乙醇(10mL)悬浮液中,然后在室温下加入3a(1.15g,4.75mmol)25分钟。在50-55℃下搅拌1小时。通过TLC监测反应进程。反应完成后,将水(10mL)加入到反应混合物中,用乙醚(20mL)萃取产物四次。合并有机层,用无水硫酸钠干燥,减压蒸发,得到固体残余物。用柱色谱(乙酸乙酯:己烷3:7)进一步纯化,得到两个肉桂酸甲酯衍生物,为E-和Z-的3.5:1混合物。同分异构体,分别为。
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