【作者】 张智泉；

【导师】 张国亮；

【作者基本信息】 天津大学 ， 生物医学工程， 2004， 硕士

【摘要】 α，α－二甲基对溴苯乙酸是一种新型的有机合成中间体，广泛应用于制药方面。本论文对溴苯乙腈甲基化-水解法合成α，α－二甲基对溴苯乙酸的工艺进行了重要改进，主要研究内容包括：1．甲基化：采用相转移催化的原理，以氯甲烷代替碘甲烷作为甲基化剂，成功的合成出了α，α－二甲基对溴苯乙腈，分析了碱（氢氧化钠）、相转移催化剂（三辛基氯化铵）及水的用量及其配比等因素对甲基化收率的影响，通过实验确定了甲基化反应的较优工艺条件，即投料配比：对溴苯乙腈：氢氧化钠：水：三辛基氯化铵：甲苯=1：0.817：0.817：0.020：3.467（质量）。在该条件下，甲基化反应的平均收率为98.75%，比文献报道值（94%）高出4.75个百分点。2．水解反应：较系统的研究了水解过程中氢氧化钾、水、乙醇等的用量及其配比等因素对水解反应时间和收率的影响，获得了较优的工艺条件，α，α－二甲基对溴苯乙酸的收率收率接近文献报道的水平。本研究为工业上制备α，α－二甲基对溴苯乙酸提供了新的方法和实验依据。更多还原

【Abstract】 In this paper, 4-bromo-α，α－dimthylbenzenacetic acid was prepared starting from 4-bromophenylacetonitrile by the methods of methylation and then hydrolyzation. In the first step, 4-bromo-α，α－dimthylbenzeneacetonitrile was successfully synthesized from 4-bromophenylacetonitrile by the methylation in accordance with the principle of phase transfer catalysis, in which catalyst was methyltrioctyl ammonium. At the same time, the effects of some factors, such as the amount of sodium hydroxide, methyltrioctyl ammonium chloride, water, and their feed ratio used in the methylating process, on the yield of 4-bromo-α，α－dimthylbenzeneacetonitrile were discussed, and the better methylating conditions were determined. It was shown that both the yield and purity of 4-bromo-α，α－dimthylbenzeneacetonitrile are higher than those reported in the literature by the other method.In the step of hydrolyzation, we studied systematically the factors affecting the reaction time and yield of hydrolyzation, such as the amount of potassium hydroxide, ethanol, water and their feed ratio. The better process conditions were obtained, and the yield was close to those reported in the literature. The present study provided a new method of synthesizing the title compound, and it had importance in the industrial production of 4-bromo-α，α－dimthylbenzeneacetic acid.更多还原