5,7-二硝基-8-羟基喹哪啶合成工艺研究

Study on Synthetic Process of 5,7-dinitro-8-hydroxy-2-Methylquinoline

实验以8-羟基喹哪啶为底物,混酸为硝化剂合成5,7-二硝基-8-羟基喹哪啶。考察了反应温度、反应时间和混酸体积比对产物收率的影响。实验结果表明,其最佳反应条件:8-羟基喹哪啶、硝酸和浓硫酸的物质的量投料比为1∶2.7∶13.9,反应混合物在温度为-5℃(温度精确到±1℃)下先反应3h,然后,室温下反应1h,经真空抽滤、氨水中和及甲醇重结晶等后处理得黄色针状晶体,纯度98.65%,收率82%。产物的结构用红外光谱和氢核磁共振谱进行了表征。

5,7 - dinitro - 8 - hydroxy - 2 - methylquinoline was synthesized from 8 - hydroxy - 2 - methylquino- line and a mixture of nitric acid with concentrated sulfuric acids. The optimun conditions were found as follows： raw material molar ratio of 8- hydroxy-2- methylquinoline, nitric acid and concentrated sulphuric acid 1：2.7： 13.9. The mixture was reacted for 3 hours at -5°C, and I hour in room temperature, with the product yield of 82 % and the purity of 98.65%. The structure of the product was characterized by IR and 1H NMR.