摘要
以丙炔醇为原料,经三氧化铬氧化生成丙炔醛后,直接与苯胺反应简便地合成了β-苯胺基丙烯醛缩苯胺.通过正交实验的方法优化了反应条件,得出最佳反应条件为:6.3 mL(0.10 mol)丙炔醇中加入8.5 g(0.085 mol)三氧化铬的硫酸水溶液,氧化反应2 h后,有机相在冰浴(200 mL)冷却下再与25 mL(0.25 mol)苯胺和63 mL 10%盐酸反应得到β-苯胺基丙烯醛缩苯胺盐酸盐,收率为48.4%.将该盐酸盐溶于甲醇与氢氧化钠溶液作用得β-苯胺基丙烯醛缩苯胺.
A facile method is presented for synthesis of malonaldehyde dianil from propargyl alcohol by oxidizing using chromium trioxide and addition reaction with aniline. The best reaction condition is obtained by orthogonal tests. 6.3 mL （0.10 mol） propargyl alcohol is oxidized with 8.5 g （0.085 mol） chromium trioxide. After oxidizing for two hours, the organic layer is separated and diluted with 200 mL water. 25 mL （0.25 mol） aniline and 63 mL 10% hydrochloric acid are added, respectively, under the ice-bath condition. The yield of malonaldehyde dianil hydrochloride is 48.4%. The malonaldehyde dianli is obtained by dissolving β-malonaldehyde dianil hydrochloride in methanol and reacting with solution of sodium hydroxide.
出处
《陕西师范大学学报（自然科学版）》
CAS
CSCD
北大核心
2005年第4期75-77,共3页
Journal of Shaanxi Normal University：Natural Science Edition
基金
教育部重点科学技术研究项目(105153)
陕西省自然科学基金资助项目(2004B06)
