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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
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