节点文献
TNAZ中间体(Ⅱ)的合成及表征
Synthesis and characterization of TNAZ intermediate(Ⅱ)
【摘要】 以3-叔丁基-5-羟甲基-5-硝基四氢-l,3-噁嗪为原料,以水为溶剂,经酸性水解合成了TNAZ中间体(Ⅱ)2-叔丁氨甲基-2-硝基-l,3-丙二醇盐酸盐,并通过红外光谱、核磁共振和元素分析对其结构进行了表征。讨论了溶剂种类、水用量、盐酸用量、温度和时间对收率的影响。确定了最佳合成工艺条件为:当n(3-叔丁基-5-羟甲基-5-硝基四氢-l,3-噁嗪)∶n(HCl)∶n(H2O)=1∶3.6∶20,控温35~45℃反应9h、55~60℃反应11h,产物纯度为98%,收率为95%。
【Abstract】 TNAZ Intermediate(Ⅱ)2-Tert-butylaminamethyl-2-nityl-l,3-propanediol hydrochloride was synthesized with 3-tert-butyl-5-nitro-tetrahydro-1,3(4H)-oxazine as materials,water as solvent by acid hydrolysis,The yield of TNAZ Intermediate(Ⅱ) was 95. 0 % on defilite conditions. The conditions were as follows :n(3-tert-butyl-5-nitro-tetrahydro-1,3(4H)-oxazine)∶n(HCl)∶n(H2O)=1∶1∶3.6∶20,35℃~45℃/9h,55℃~60℃/11 h.The product was characterized by IR,HNMR,CNMR and element alanalysis.
- 【文献出处】 化学工程师 ,Chemical Engineer , 编辑部邮箱 ,2014年09期
- 【分类号】O621.3
- 【下载频次】75