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路线2:
步骤: A. 1,4,7-三(对甲苯磺酰基)-1,4,7-三氮杂庚烷的合成:在0℃下向搅拌的对甲苯磺酰氯(618g,3.24mol)的吡啶(1500ml)溶液中加入1,4,7-三氮杂庚烷(95.5g,0.926mol)的吡啶溶液(150μl),在干燥的氩气氛下,保持温度<= 50℃,加入需要30分钟,将混合物缓慢冷却至室温并搅拌3小时后,将H₂O(2升)缓慢加入冷却的(冰浴)混合物中,将形成的重白色沉淀物过滤并用H₂O彻底洗涤,将浅黄色固体溶于DMF(3升)中,并在5℃下缓慢加入0.1N HCl(4升),将浆液过滤并变为浅色用H₂O彻底洗涤黄色固体并真空干燥得到产物。
条件: With hydrogenchloride In pyridine; N,N-dimethyl-formamide
产率: 93%
参考文献: [1] Patent: US5874421, 1999, A [2] Patent: US5610293, 1997, A