摘要
为了提高产率,以对乙酰氨基酚和三氯硫磷为原料采用酰胺水解法合成了硫代磷酸三(4-氨基苯)酯,通过实验得到了合成的最佳工艺条件:各原料物质的量之比为n(对乙酰氨基酚)∶n(三乙胺)∶n(三氯硫磷)=3.10∶3.80∶1,反应温度为35℃,反应时间为3.5h.红外光谱、核磁共振谱、质谱和高效液相色谱等手段对产品进行了结构表征.通过对实验方法的进一步研究,结果发现在三乙胺中加入少量的吡啶,组成复式缚酸剂后,能有效地提高反应的产率.在此优化工艺条件下,产率为84%.
For improving the product yield,tris（4-aminophenyl） thiophosphate was synthesized from acetaminophen and thiophosphoryl chloride by amide-hydrolyzing process. The optimum reaction conditions obtained by experiments：ere the mole ratio of acetaminophen triethylamine∶ thiophosphoryl chloride of 3.10∶3.80∶1,the reaction temperature of 35 ℃ and the reaction time of 3.5 h. The structure of the product was characterized by IR,NMR,MS and HPLC. Further study on the experiment shows that the addition of a small amount of pyridine into triethylamine can improve the yield of the reaction effectively. Under the optimum reaction conditions,the yield of reaction reaches 84%.
出处
《材料科学与工艺》
EI
CAS
CSCD
北大核心
2009年第6期797-800,共4页
Materials Science and Technology
基金
国家自然科学基金资助项目(50472048)
关键词
酯化
水解
合成
硫代磷酸三(4-氨基苯)酯
esterification hydrolysis synthesis tris（4-aminophenyl） thiophosphate
