Chemistry
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通过超硫酸盐促进的β、β-不饱和化合物和烷基奈的苯基的高效合成在水中的多功能苯
Chapters
Summary
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报道了水中对β、β-不饱和化合物和烷基化合物的超硫酸盐促进的无金属苯化，以合成前所未有的多功能化苯。
Transcript
这是一个非常简单的实验设置，符合有机化学要求，以获得一系列可行的多功能苯。该技术的主要优点是使用水作为溶剂，使粗混合物易于分离，并有助于有机化学的可持续实践。证明这个程序的将是加布里埃拉·苏扎博士，一个来自我实验室的副研究员。
首先，在含有搅拌棒的15毫升试管中加入两毫升蒸馏水。按顺序添加220微升乙二苯酚、96.8微升2环氧1-1、1.5毫升新鲜准备的1.3摩尔铵。使用橡胶隔膜盖住管子，并在管内插入针头，以避免在加热过程中最终积聚压力。
将管子放在热板上的铝加热块中，在 1，150 RPM 的剧烈搅拌下，在 85 摄氏度下加热 8 小时。。为了允许反应的进展，采取反应介质的50微升等同，并转移到1.5毫升锥形小瓶。在小瓶中加入50微升乙酸乙酯并摇动。
然后用毛细管收集有机顶层，并将其涂在TLC硅涂层玻璃板上。将板浸入92：8乙酸乙基溶液中进行分析。将反应混合物冷却至室温，并在试管中加入一毫升乙酸乙酯。
搅拌悬架约一分钟，然后在室温下以 2，336 次 g 离心，进行一分钟。使用巴斯德移液器去除有机顶层，并将其转移到圆形底部烧瓶中。重复添加乙酸乙酯到离心和去除顶层两次。
使用旋转蒸发器在减压下将顶层集中，以获得原油。以92：8的比例加入55毫升六烷和乙酸乙酯混合物，放入含有7.5克二氧化硅的烧杯中。搅拌烧瓶以获得均匀的浆料。
将泥浆转移到内径为 40 毫米的柱上，以包装柱子。将原油溶解在少量的乙酸乙酯中，然后将溶液转移到柱子上。在试管中收集柱污水。
执行 TLC，根据仅显示一种迁移化合物的 TLC 结果获得所需的纯产品。在旋转蒸发器上降低压力下将所需溶液集中，并在高真空下去除最终挥发性液体至少一小时。使用脱化氯仿分析质子和碳-13 NMR纯化产品的样品。
在此协议中，多甲苯被分离为无色油。在质子和碳-13 NMR光谱中评估了结构和纯度。8.37 和 7.72 PPM 中央苯环上的芳香质子峰值用作产品形成诊断信号。
仔细控制反应介质的温度，确保反应过程中适当搅拌悬浮液非常重要。此过程可用于在水中进行的任何其他转化。保持工作步骤是从反应介质获得粗混合物的一种有效方法。
该程序提供了一种简单而有效的方法来研究水作为反应介质，并鼓励设计更可持续的转化。为了操作安全，在用橡胶隔膜盖住管子后，在加热前一定要插入针头。它避免在反应过程中积聚任何压力。
Tags
化学， 问题 154， 苯，在水有机反应， 渗透， 多功能化苯， 无金属反应， β， β-不饱和化合物， 烷基Related Videos
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