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摘要：以苯甲醛为原料，维生素B1作为催化剂，发生缩合反应生成安息香，经过氧化得到二苯基乙二酮，然后与尿素环合反应合成苯妥英钠。通过改变苯甲醛缩合反应的反应条件合成安息香，薄层色谱跟踪实验进程合成二苯乙二酮，并用红外光谱和核磁共振谱对产物进行表征。结果表明，反应的优化条件为：蒸过的苯甲醛与催化剂在冰水中磁力搅拌1.5h，然后水浴温度上升到50 ~ 60度，继续搅拌1.5h，继续升温，水浴温度控制在85℃左右，在此条件下，安息香收率可达79%，安息香氧化制备二苯乙二酮的反应时间为4h，苯妥英钠收率可达45.45%。68766
毕业论文关键词：苯甲醛；维生素B1；安息香；苯妥英钠
Preparation and Study of Phenytoin Sodium
Abstract: Benzene formaldehyde as raw material，VB1 as a catalyst， in the alkaline environment by benzoin condensation，oxidation and a series of reactions synthesis of phenytoin sodium. Finally, under alkaline conditions, the reaction of diphenylethanedione with urea to obtain phenytoin， and then with sodium hydroxide react with sodium salt, that is phenytoin sodium. The optimized reaction scheme was selected by changing the reaction conditions of benzoin condensation， and the prepared product was characterized by IR and 1H-NMR. The results showed that the optimized conditions were as follows: the crude benzaldehyde and the catalyst were heated to 50 ~ 60 ℃ after 1.5 h reaction with ice water. The reaction was continued for 1.5 h，the temperature was raised to 80 ~ 90 ℃. Under these conditions， the yield of benzoin can reach 79%，the reaction time of benzodiadione prepared by benzoin oxidation was 4h,phenytoin sodium of 45.45% was obtained.
Keywords: Benzaldehyde; Vitamin VB1; benzoin; Phenytoin sodium
目录
1 绪论 1
1.1 开题依据 1
1.2.1安息香的合成 1
1.2.2二苯乙二酮的合成 3
1.2.3苯妥英钠的合成 4
1.3 方案论证 4
1.3.1苯妥英钠的制备 5
2 实验部分 6
2.1 仪器与试剂 6
2.1.1 仪器 6
2.1.2 试剂 7
2.2 反应装置图 7
2.3 化学反应与机理 9
2.4 有机合成实验步骤 10
2.4.1 安息香的制备 10
2.4.2 二苯乙二酮的制备 11
2.4.3 苯妥英钠的制备 11
2.5 薄板层析跟踪反应实验步骤 11
2.5.1 硅胶板的制备 12
2.5.2 硅胶板的活化与点样 12
2.5.3 显色与计算 12
3 结果与讨论 13
3.1 安息香的制备研究 13
3.2 二苯乙二酮的制备研究 14
3.3 苯妥英钠的制备研究 16
3.4 谱图分析 16
4 结论 21
致谢 22