3,3,3-三甲氧基丙腈的合成与表征 |
| |
引用本文: | 王丽娜,陈春光,陈学玺. 3,3,3-三甲氧基丙腈的合成与表征[J]. 湖北化工, 2012, 0(3): 57-60 |
| |
作者姓名: | 王丽娜 陈春光 陈学玺 |
| |
作者单位: | [1]青岛科技大学化工学院,山东青岛266042 [2]天津大学化工学院,天津300072 |
| |
摘 要: | 以丙二腈为起始原料通过两步反应合成了3,3,3-三甲氧基丙腈,气相色谱分析产物纯度达到98.08%。采用气质联用、红外光谱、核磁共振氢谱对产物进行了表征。确定了第一步合成甲基氰基乙酰亚氨基盐酸盐的最佳反应条件为:溶剂含水量〈100×10-6^、通气时间3h、72g丙二腈、45mL甲醇、1440mL乙醚、常温搅拌时间7h;第二步合成3,3,3-三甲氧基丙腈的最佳反应条件为:甲基氰基乙酰亚氨基盐酸盐与甲醇的物料比为1g:7.35mL、搅拌时间24h、在反应i0h后移出副产物氯化铵、无水硫酸钠作为干燥剂。
|
关 键 词: | 3 3 3-三甲氧基丙腈 医药中间体 合成 表征 |
Synthesis and Characterization of 3,3,3-Trimethoxypropanenitrile |
| |
Affiliation: | WANG Li-na, CHEN Chun-guang , CHEN ( College of Chemical Engineering ,Qingdao University of Qingdao 266042 ,China ; Xue-xP Science and Technology, College of Chemical Engineering, Tianjin University, Tianjin 300072, China) |
| |
Abstract: | 3,3,3-Trimethoxypropanenitrile was synthesized after two-step reactions by using malononitrile as raw material. Through the analysis of gas chromatography, the product purity reached 98.08%. GC-MS, IR and 1HNMR were applied to the product characterization. The optimum reaction conditions of the first step to synthesize methyl cyanoacetimidate hydrochloride were determined as follows:water content of solvent less than 100 X 10-6, ventilation time of 3 h, malononitrile amount of 72 g, methanol amount of 45 mL, ether amount of 1440 mL, stirring for 7 h at room temperature. The optimum reaction conditions of the second step to synthesize 3,3,3-trimethoxypropanenitrile were as follows:the ratio of methyl cyanoacetimidate hydrochloride to methanol of 1 g : 7.35 mL, stirring time of 24 h,removing ammonia chloride after reacted for 10 h,using anhydrous sodi- um choloride as drying agent. |
| |
Keywords: | 3 3 3-trimethoxypropanenitrile medicine intermediate synthesis characterization |
本文献已被 维普 等数据库收录! |
|