金雀异黄酮甲基化合成樱黄素的工艺研究

Synthesis of Prunetin from Genistein Methylation

以金雀异黄酮为原料,经碘甲烷甲基化合成樱黄素。研究了溶剂、反应物配比、反应时间、重结晶溶剂对反应的影响。优化条件为:N,N-二甲基甲酰胺溶剂、n(金雀异黄酮)∶n(碘甲烷)∶n(碳酸钾)=1.0∶4.0∶0.5、反应8 h、乙腈为重结晶溶剂,收率81.0%。放大后以85.1%的收率制得145.0 g产品。

Using genistein as starting material, prunetin was synthesized via methylation by iodomethane. The reaction conditions were evaluated. A yield of 81.0% was achieved under the optimal conditions including N,N- Dimethylformamide as solvent, n（genistein）：n（iodomethane）：n（potassium carbonate）=1.0：4.0：0.5; reaction time of 8 h, acetonitrile as recrystallization reagent.