增感剂9-苯基吖啶的合成研究

Synthesis of 9-phenylacridine

吖啶类化合物是重要的精细化工产品,在材料、化工、生物、制药领域应用广泛。以N-苯基邻氨基苯甲酸为起始原料合成吖啶酮,与格氏试剂反应生成9-羟基-9-苯基吖啶,再经还原合成标题化合物。研究结果表明:以多聚磷酸为催化剂合成吖啶酮,收率89.2%,纯度>98%;格氏试剂与吖啶酮反应条件温和,9-羟基-9-苯基吖啶收率65%,纯度>98%;9-羟基-9-苯基吖啶经次亚磷酸钠还原得9-苯基吖啶,收率约为91.5%,纯度>98%。实验中采用LC-MS、1HNMR、HPLC等分析方法对各反应产物进行结构确定和纯度测定。

Acridine compounds are important chemical intermediates and widely applied in the material, chemical, biologi- cal and pharmacy fields. In this work, the N-phenylanthranilic acid were used as the starting materials to syntheze acri- danone. Then the product （I） was synthesized by acridanone and grignard reagent. Finally, 9-phenylacridine was prepared by reduction reaction. The results indicated that in the presence of polyphosphoric acids,the yield of acridanone was more than 89. 2% and the purity was up to 98%. Moreover, the yield of product（I） was more than 65% and the purity was up to 98%. The yield of 9-phenylacridine was more than 91.5% and the purity was up to 98% when synthesized via sodium hypophosphite monohydrate. The products and in- termediates were confirmed by LC-MS, 1HNMR, GC and HPLC.