作为有机合成中间体,用于构建复杂分子结构,在医药和农药研发中发挥关键作用。
医药; 农药
合成路线 1(1. 合成:128376-64-7)
产率:95%
合成条件:With bis-triphenylphosphine-palladium(II) chloride; potassium acetate In 1,4-dioxane at 80℃; for 15 h; Inert atmosphere
实验步骤:向搅拌的化合物Z 1(2c 8g,0.15mol),化合物2,2(45.7g,0.18mol)和PdCa(PPha 2)(5.26g,7.5mmof)在1,4-二恶烷中的溶液( 在氩气氛下加入KOAc(22.0×0.225mol),在80℃下搅拌混合物15分钟,减压除去溶剂,用PE(500nL)稀释残余物。 通过过滤除去,并将滤液在减压下浓缩,得到粗产物,将其通过快速色谱法(硅胶/ FE:EA 1 Q-1)纯化,得到4-(4t4,5,5-四甲基-1,3.2)。 - 二氧杂环戊烷-2-基)ben2aid©hyd(2.3,32.5g,95%),为白色固体。
参考文献:
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合成路线 2(2. 合成:128376-64-7)
产率:91%
合成条件:at 20℃; for 2 h;
实验步骤:向4-甲酰基苯基硼酸(1g)的无水THF(10mL)溶液中加入2,3-二甲基 - 丁烷-2,3-二醇(0.867mg),将该混合物在室温下EPO搅拌2小时。。 将溶剂蒸发至干。 将残余物溶于二氯甲烷(40mL)中,用水(25mL×3)洗涤,干燥并真空蒸发,得到4-(4,4,5,5-四甲基 - [1,3,2]二氧杂硼杂环戊烷 - 2-基) - 苯甲醛(1.41g,91%收率)。 1H-NMR(400MHz,CDCl3):δ1.34(s,12H,4CH3),7.86(d,J = 8.4Hz,2H,H-Ar),7.96(d,J = 8Hz,2H ,H-Ar),10.05(s,1H,CHO)ppm。
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