【摘要】 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%。更多还原

【Abstract】 Tri( 4-hydroxyphenyl) ethane was synthesized from acetylacetone and phenol in the presence of p-toluene sulfonic acid( p-TSA) and 3-mercaptopropionic acid as the catalysts. The structure was confirmed by IR and1HNMR. The synthesis conditions are investigated by single-factor experiment. Five factors such as material ratio,usage of main catalyst,usage of cocatalyst,reaction temperature and reaction time were studied and the results show that its maximum yield is obtained under the following conditions: the molar ratio of phenol and acetylacetone is 9∶ 1,the mass ratio of p-TSA and acetylacetone is 1 ∶ 1,the mass ratio of 3-mercaptopropionic acid and acetylacetone is 1 ∶ 7,the reaction temperature is 55 ℃ and the reaction time is 24 h. The yield of product is up to 78%. The purification process was also investigated and purity was close to 100%.更多还原