声化学法制备格利雅试剂及其合成二甲基苄基甲醇的研究

【作者】 漆小龙；

【导师】 邓淑华；

【作者基本信息】 广东工业大学 ， 化学工艺， 2004， 硕士

【摘要】 二甲基苄基甲醇是一种重要的香料，它除了可用于制备花香型香精，如百合，水仙，铃兰等高级花香型香精外，它的乙酸酯有清新的香韵，因而使其价值倍增，常用在风信子，百合，茉莉花等花香型香精中。 格利雅试剂在香料、医药的合成中应用很广泛，但传统的制备工艺要求苛刻。本研究采用的在超声波条件下制备格利雅试剂，工艺简单，反应时间大大缩短，对设备的要求低，条件温和，反应可以用普通试剂级的乙醚或THF而无需干燥，且不需要对周围环境的条件提出严格要求，反应的诱导期大大缩短，可直接得到高产率的格利雅试剂，而且相当一部分较难合成的格利雅试剂在超声波条件下合成时不需要引发剂。这些对格利雅试剂的工业化生产具有重要的意义。 本文探讨了超声波合成格利雅试剂的机理，研究了声化学法制备格利雅试剂氯化苄基镁的最佳工艺条件为：在超声波的功率为500W，频率为25KHZ，有12个换能器的条件下，水浴温度为20℃，以THF为溶剂，不搅拌。 本论文首次利用声化学法制备格利雅试剂-氯化苄基镁，并研究了利用氯化苄基镁合成二甲基苄基甲醇的原理及最佳工艺条件，其工艺条件为：丙酮的浓度为12.5％，丙酮与格利雅试剂的摩尔比为1：1.1，温度为10℃。 主要研究内容如下： 1．探讨了超声波合成格利雅试剂的机理 2．研究超声波法制备格利雅试剂氯化苄基镁的工艺条件。探索合成格利雅试剂的新工艺。 3．研究二甲基苄基甲醇制备方法，寻找制备二甲基苄基甲醇的最佳工艺条件和工艺路线。更多还原

【Abstract】 Dimethylbenzyl carbinol is a kind of important spices, it not only can be used for preparing the fragrant essence of flower, for instance lily, the advanced fragrant essence of flower, the narcissus , the lily of the valley ,etc., but also Dimethylbenzyl carbinol acetate have fresh fragrant and it make it’s value double. Dimethylbenzyl carbinol acetate usually used in the fragrant essence of flower of hyacinth, lily, jasmine etc..Grignard reagents are used very extensive in being synthetic in spices, medicine. The traditional preparation craft requests were rigor. Under ultrasonic, the craft of preparation Grignard reagents is simple, reactive time being shorten greatly, only needing simple equipments, mild condition and the reactive impregnant can used ordinary ether or THF that can not need to be dry. Reactive induction period shorten greatly, Grignard reagents of high yield rate can get directly and quite a few Grignard reagents that more difficult to preparation did not need initiator while synthesized under the ultrasonic condition. It has important meanings in industrialization of Grignard reagents.This paper has probed into the synthetic mechanics of Grignard reagents under ultrasonic condition. This paper has studied preparation of Grignard reagents under phonochemistry and optimum technologic conditions is: the power of ultrasonic is 500W and frequency is 250KHZ, having twelve energy conversion devices, water bath temperature being 20C, solvent being THF,unstirred.This paper first prepared Grignard reagent benzylmagnesium chloride under phonochemistry and we have researched the principle and optimum technologic conditions while used benzylmagnesium chloride preparation Dimethylbenzyl carbinol .The optimum technologic conditions is: the concentration of acetone being 12.5 percent, mol ratio being 1.1:1 between acetone and Grignard reagent, temperature being 10C.The main research contents are as follows:1. Discuss mechanism of preparing Grignard reagents under ultrasonic condition.2. Study the technologic conditions of preparing Grignard reagent benzylmagnesium chloride under ultrasonic condition. Explore the new craft of preparing Grignard reagents.3. Study prepared method of dimethylbenzyl carbinol and seek the best technologic conditions and craft route of dimethylbenzyl carbinol.更多还原