1,2,3-苯三氧基三乙酸的相转移催化合成

以三丁基乙基硫酸乙酯铵作催化剂,以三氯甲烷作溶剂,采用连苯三酚和一氯乙酸为原料在氢氧化钠存在的条件下,合成了1,2,3-苯三氧基三乙酸.研究了催化剂的种类和用量对反应的影响,并通过正交试验,得到了1,2,3-苯三氧基三乙酸的最佳合成条件连苯三酚0.05mol,三丁基乙基硫酸乙酯铵与连苯三酚的量比为150,一氯乙酸与连苯三酚的量比为3.31,氢氧化钠与连苯三酚的量比为7.01,溶剂CHCl3的用量为100.mL,溶剂回流温度下反应时间1.5h.在上述反应条件下,产物的产率达到90.5%(质量分数).此外,分析了1,2,3-苯三氧基三乙酸的红外光谱特征.

Synthesis of 1,2,3-phenyltrioxyl tri by phase-transfer catalysis

1,2,3-phenyltrioxyl tri (acetic acid) (PTAA), which was generally prepared from pyrogallol and chloroacetic acid in an alkali solution, can be synthesized with a high yield by the catalysis of tributylethylammonium ethosulfate in chloroform solvent. The effect of different catalysts was investigated and tributylethylammonium ethosulfate was chosen for its high performance, of which the amount was optimized to be 1:50. The reaction conditions of synthesis were optimized as follows: the molar ratio of chloroacetic acid to pyrogallol 3.3:1, sodium hydroxide 7.0:1, solvent chloroform 100mL and reaction time 1.5 h under solvent reflux temperature. In these conditions, the yield may reach 90.5% PTAA. IR spectrum of PTAA was developed and studied.