化学合成。
化学合成
合成路线 1(1. 合成:660867-80-1)
产率:39%
合成条件:With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate In 1,4-dioxane at 80℃; for 4 h; Inert atmosphere; Sealed tube
实验步骤:向先前脱气的4-溴-2-甲基哌啶(0.500g,2.906mmol),4,4,4',4',5,5,5',5'-八甲基-2,2'-二(4)的脱气溶液( 在50mL密封管中加入1,3,2-二氧杂硼杂环戊烷(0.812g,3.997mmol),乙酸钾(0.854g,8.720mmol)的1,4-二恶烷(5mL)溶液[1,1'-双(二苯基膦) 二茂铁]二氯化钯(II)(0.021g,0.029mmol)并在80℃下搅拌4小时。 蒸发掉溶剂并在硅胶上纯化柱色谱(乙酸乙酯:乙醚= 3070),得到标题化合物(0.250g,39%),为灰白色固体.LCMS:m / z 220.1 [M + H]。
参考文献:
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