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为了提高标题化合物THPE的产率、简化操作过程,以苯酚和乙酰丙酮为原料,选用对甲苯磺酸和3-巯基丙酸作催化剂,合成了标题化合物;采用红外光谱分析、1HNMR和液相色谱对标题化合物的结构和纯度进行了表征。通过单因素试验,考察了原料配比、主催化剂用量、助催化剂用量、反应温度和反应时间对产率的影响,得出标题化合物的最佳合成工艺为:n(苯酚)∶n(乙酰丙酮)=9∶1;m(对甲苯磺酸)∶m(乙酰丙酮)=1∶1;m(3-巯基丙酸)∶m(乙酰丙酮)=1∶7;反应温度55℃;反应时间24 h;THPE粗产品产率稳定在78%以上。同时对其纯化处理进行了研究,1次CH2Cl2和4次乙醇/水提纯后产品的纯度达到了99.86%。
In order to improve the yield of the title compound THPE and simplify the process, the title compound was synthesized by using p-toluenesulfonic acid and 3-mercaptopropionic acid as starting materials and phenol and acetylacetone as raw materials. The compounds were characterized by IR, 1HNMR and LC The structure and purity of the title compound were characterized. Through single factor experiments, the effects of the ratio of raw materials, the amount of procatalyst, the amount of cocatalyst, the reaction temperature and the reaction time on the yield were investigated. The optimum synthesis conditions of the title compound were as follows: n (phenol): n ) = 9: 1; m (p-toluenesulfonic acid): m (acetylacetonate) = 1: 1; m (3- mercaptopropionic acid): m 24 h; THPE crude product yield was stable at above 78%. At the same time, the purification of the product was studied. The purity of the product reached 99.86% with one pass of CH2Cl2 and four times of ethanol / water purification.