摘要
以1-硝甲基环己醇（1-NMCH）为主要原料，经过铁粉还原、重氮化、扩环反应制得了环庚酮。利用气相色谱对产品进行纯度测定并且通过红外光谱、核磁共振对产品结构进行了表征。探讨了反应条件对产品产率的影响，找出了较佳的合成工艺条件。结果表明合成较佳工艺条件为：铁粉与1-NMCH摩尔比为3．5：1．0，铁粉还原的PH值范围为5～6，还原温度为40℃，重氮化温度为5℃以下，重氮化PH值范围为4～5，产品产率为48．69％．
The cycloheptanone was synthesized with the main material 1-（Nitromethyl） -cyclohemanol through iron reduction, diazotization and ring expansion reaction. The purity of samples by GC spectrum was determined and the structure was characterized by IR spectrum and H-NMR spectrum. The effects of the synthesis conditions on the yield of product were discussed, with much better synthesizing process found. The results indicate that the optimal synthesis conditions are as follows： the molar ratio of iron powder to 1-（nitromethyl） -cyclohemanol is 3.5：1.0, the control range of iron reduction PH is 5～6, the temperature of iron reduction is 40℃ the temperature of diazotization is below 5℃, the control range of diazotization PH is 3～4. The yield of products is 48.69%.
出处
《辽宁工业大学学报（自然科学版）》
2012年第6期401-404,共4页
Journal of Liaoning University of Technology(Natural Science Edition)
关键词
1-硝甲基环己醇
环庚酮
还原
重氮化
l-（nitromethyl）-cyclohemanoi
cycloheptanone
reduction
diazotization
