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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-dimethylhydantoin (BBDMH) was synthesized from 5, 5-dimethylhydantoin (DMH) and 1,4-dibromobutane and purified by column chromatography Purification by method, followed by TLC. The products were characterized by Fourier transform infrared spectroscopy (FTIR), 1HNMR, 13CMR, XRD and elemental analysis. The effects of the species of acid-binding agent, reaction time, molar ratio of materials and reaction temperature on the yield of BBDMH were studied. On the basis of single factor experiments, the synthesis process was optimized by using the Box-Behnke experimental design in response surface analysis. The optimal conditions for the preparation of 3-bromobutyl-5,5-dimethylhydantoin were as follows: the acid-binding agent was anhydrous K2CO3 and its mass ratio to DMH was 4:1, the reaction temperature was 50 ℃, n (1, 4-dibromobutane) / n (DMH) = 2.67, the reaction time is 4.40 h. Under these conditions, the yield was 92.89%, which was close to the regression model and the relative error was only 0.25%.