摘要
过渡金属催化的偶联反应是形成碳-氮键最为有效的手段之一,己经被广泛地应用于有机化学的许多领域。近年来对偶联反应的研究和报导层出不穷,主要集中在寻找新的催化剂,配体和催化体系进行反应,扩大反应的应用领域。采用过渡金属催化有机反应来构建C-N键是一种有效的合成策略。铜催化剂具有价格便宜、低毒等优点,因而近年来受到广泛的关注。本论文以过渡金属催化的碳-氮键偶联反应为研究内容,为了得到最优的反应条件,首先考察水介质中各种铜催化剂(Cu、CuO,Cul,CuBr,CuCI,Cu(0Ac)_2,CuBr_2等)对反应的催化性能,筛选出具有较好催化活性的铜催化剂,然后,考察常见配体和铜催化剂对反应的影响,并从催化剂用量、物料比、温度、压力、反应时间、原料混合程度等方面来探索水介质中碳氮键构建反应的技术路线。在产物的分离与表征中,用薄层液相色谱和柱色谱分离合成中间体以及目标产物,采用傅立叶如外光谱来表征中间体和目标化合物的特征吸收峰,核磁共振氫谱(1HNMR)、破谱(13CNMR)来表征目标化合物结构特征。
Transition metal catalyzed coupling reaction is One of the most effective means of formation of carbon - nitrogen keys, has been widely used in manyfields of organic chemistry. Dual reaction in recent years studies and reports emerge in endlessly, mainly concentrated in the search for new catalyst, Gilligan and system of catalytic reaction, application field of expanding reaction. Transition metal catalyzed organic reactions is used to build the C - N key is a kind of effective synthetic strategy. Copper catalyst has the advantages of cheap, low toxicity, thus attracted much attention in recent years. First investigation of various copper catalyst on reaction in aqueous medium is catalytic properties, filter has a good catalytic activity of copper catalyst, then, makes a research on the common Gilligan and copper catalyst reaction, and from the catalyst, material ratio, temperature, pressure, reaction time, and degree of raw materials mixing to explore water medium carbon and nitrogen key building response technical route. In the separation and characterization of the product, with a thin layer of liquid cartographic and column cartographic separation of intermediates and target product, USES the Fourier infrared spectrum characteristic absorption peaks of the intermediates and target compounds in the characterization, nuclear magnetic resonance hydrogen spectrum (1 h NMR), carbon (13 c NMR) characteristics of the target compound was characterized by structure.
出处
《当代化工研究》
2016年第9期150-151,共2页
Modern Chemical Research
关键词
铜催化
碳氮偶联
过渡金属
copper catalyst
carbon and nitrogen coupling
transition metal