摘要
通过两步反应制备了2,4,6-三(4-甲基苯基)-1,3,5三嗪。首先以碘作为引发剂,对溴甲苯和镁在四氢呋喃溶液中加热回流制得对甲苯基溴化镁。第二步将对甲苯基溴化镁在冰水浴及Ar充分保护下与三聚氯氰反应得到2,4,6-三(4-甲基苯基)-1,3,5三嗪,最后经重结晶得到纯度较高的2,4,6-三(4-甲基苯基)-1,3,5三嗪。通过对产物的核磁共振氢谱、碳谱和红外光谱分析,确定所得产品即为2,4,6-三(4-甲基苯基)-1,3,5三嗪,产率约为40.6%。
In this thesis, 2,4,6-tris(4-methylphenyl) -1,3,5-triazine was synthesized by two step reactions. In the first step, Grignard reagent was produced under reflux condition using 4-bromotoluene and Mg as main raw materials, iodine as initiator, and tetrahydrofuran as solvent. Then the prepared Grignard reagent was cooled to about 35℃. In the second step, the cooled Grignard reagent was added into the flask under ice water bath to react with cyanuric chloride under the adequate protection of Ar to produce crude 2,4,6-tris (4-nlethylphenyl) -1,3,5- triazine. High purity product could be produced by the recrystallization of crude 2,4,6-tris (4-methylphenyl) - 1,3,5-triazine in ethyl acetate. The structure of the product was identified by nuclear magnetic resonance (NMR) analysis and fourier transform infrared spectroscopy (FTIR) analysis. The result showed that the product is 2,4,6- tris (4-methylphenyl)- 1,3,5-triazine, the yield was about 31%.
出处
《化学工程师》
CAS
2016年第7期11-13,共3页
Chemical Engineer
基金
陕西省教育厅专项科研计划项目基金(14JK1041)
陕西省教育厅重点实验室科研计划项目基金(14JS006)
陕西省重点实验室项目(2010JS069)
关键词
格氏反应
三聚氯氰
2
4
6-三(4-甲基苯基)-1
3
5三嗪
核磁共振谱
grignard reaction
cyanuric chloride
2,4,6-tris(4-methylphenyl) -1,3,5-triazine
nuclear magnetic resonance spectroscopy