异甘草素的合成工艺研究

Optimization of Synthesis Process of Isoliquiritigenin

以2,4-二羟基苯乙酮和对羟基苯甲醛为原料,通过羟基保护,羟醛缩合及脱保护合成得到了异甘草素。并对其中的关键步骤羟醛缩合反应条件如:催化剂的种类,底物的摩尔比,反应温度,溶剂以及反应时间进行了优化。结果表明,在以Ba(OH)2为催化剂,甲醇为反应溶剂,对羟基苯甲醛和2,4-二羟基苯乙酮的摩尔比为1.8∶1,温度为45℃的条件下,反应12 h,羟醛缩合反应的收率最高(77.9%),且体系较为简单,易于纯化。

Isoliquiritigenin was synthesized with 2,4-Dihydroxyacetophenone and 4-Hydroxybenzaldehyde as the starting materials by protecting of hydroxy, Aldol Addition and deprotecting. The reaction conditions of the key step-Aldol Addition, including catalyst, ratio of substrates, temperature, solvent and time were optimized. Resuits showed that the optimal condition of the key step were as follows： catalyst Ba（OH） 2, solvent MeOH, M（4- Hydroxybenzaldehyde） ： M （2,4-Dihydroxyacetophenone） = 1.8：1, tempetature 45℃, and time 12 h. Under the optimal conditions, the yield of the reaction achieved the highest（77.9% ）. In addition, the reaction system was simple and easily purified.