响应面法优化3-溴丁基-5,5-二甲基海因的制备工艺  

Using response surface methodology to optimize preparation of 3-bromobutyl-5,5-dimethyhydantoin

作　　者：郭睿[1] 李云鹏 宋博 马兰 土瑞香 王映月[1] 郭煜 GUO Rui LI Yun-peng SONG Bo MA Lan TU Rui-xiang WANG Ying-yue GUO Yu(MOE Key Laboratory of the Chemistry and Technology of Light Auxiliary Chemicals, Shaanxi University of Science and Technology, Xi＇ an 710021, China)

机构地区：[1]陕西科技大学教育部轻化工助剂化学与技术重点实验室,陕西西安710021

出　　处：《现代化工》2017年第10期105-109,共5页Modern Chemical Industry

基　　金：陕西省教育厅服务地方专项计划项目(15JF011);陕西省工业科技攻关项目(2016GY-146)

摘　　要：以5,5-二甲基海因(DMH)、1,4-二溴丁烷为原料,合成了3-溴丁基-5,5-二甲基海因(BBDMH),并以柱色谱法分离提纯,薄层色谱法跟踪产物。利用傅里叶红外光谱(FTIR)、核磁共振氢谱(1HNMR)、核磁共振碳谱(13CNMR)、X-射线衍射(XRD)、元素分析对产物进行了表征。研究了缚酸剂的种类、反应时间、物料摩尔比、反应温度对BBDMH产率的影响。并在单因素实验的基础上利用响应面分析法中的Box-Behnke实验设计对合成工艺进行优化。制备3-溴丁基-5,5-二甲基海因的最佳工艺条件:缚酸剂为无水K2CO3且与DMH的质量比为4∶1,反应温度为50℃,n(1,4-二溴丁烷)/n(DMH)=2.67,反应时间为4.40 h。在此条件下,产率为92.89%,与回归模型的预测值很接近,相对误差仅为0.25%。3-bromobutyl-5,5-dimethyl-hydantoin（BBDMH） is prepared using 5,5-dimethyl-hydantoin（DMH）and 1,4-dibromobutane as raw materials.The product is separated and purified by column chromatography method and is tracked by thin layer chromatography method. The gained BBDMH are characterized by Fourier transform infrared spectroscopy（FTIR）,H-nuclear magnetic resonance spectrum（1HNMR）,C-nuclear magnetic resonances spectrum（13CNMR）,X-ray diffraction（XRD） and elemental analysis. In addition,the effects of kinds of acid binding agent,reaction temperature,the molar ratio of 1,4-dibromobutane to DMH,and reaction time on the yield of BBDMH are investigated.Furthermore,on the basis of single factor experiment,the synthetic process is optimized by using the BoxBehnken experiment design principle in the response surface methodology. The optimal conditions for the preparation of BBDMH are as follows： anhydrous potassium carbonate is used as the acid blinding agent and its mass ratio to DMH is 4 ∶1,the reaction temperature is at 50℃,the molar ratio of 1,4-dibromobutane to DMH is 2. 67 ∶1,and the reaction time is 4h.Under these optimal conditions,the yield rate of BBDMH reaches 92. 89%,which is very close to the predictive result of the regression model with the relative error value of 0. 25%.

关 键 词：3-溴丁基-5 5-二甲基海因 柱色谱分离 工艺优化 响应面法 回归模型 

分 类 号：O622.6[理学—有机化学]