| 华川,杨晓健,刘兴丽,马培华,周清娣.化学通报,2015,78(12):1102-1107. |
| 溴甲基取代甘脲二醚的合成与晶体结构表征 |
| The synthesis and crystal characterization of bromomethyl substituted glycoluril diether |
| 投稿时间：2015-03-20 修订日期：2015-04-20 |
| DOI： |
| 中文关键词: 溴代丁二酮 最佳合成工艺 溴甲基取代甘脲 溴甲基取代甘脲二醚 |
| 英文关键词:1,4-dibromo-2,3-butanedione, the optimum technology, bromomethyl substituted glycoluril, bromomethyl substituted glycoluril diether |
| 基金项目:贵州大学国家级大学生创新性实验计划项目（2013）013号资助，教育部“春晖计划”Z2011035资助 |
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| 中文摘要: |
| 以溴代丁二酮为原料，探究溴甲基取代甘脲的最佳合成工艺，分别从加料方式、酸度、原料摩尔比等方面进行考查。其最佳合成工艺为：溴代丁二酮与尿素的摩尔比为1:5，加入水-乙醇混合溶剂，搅拌24h后，加入溶剂体积2.5%的三氟乙酸，反应时间为48h，产率达60.8%，相对文献[10]，产率提高了20%-30%。并利用溴甲基取代甘脲与多聚甲醛在氢溴酸-冰乙酸体系下75℃恒温反应1h，得溴甲基取代甘脲二醚，产率达65.5%。在利用核磁共振技术对化合物的结构及性能进行检测和表征的同时，使用X射线单晶衍射技术确定了其中两个化合物的晶体结构。 |
| 英文摘要: |
| In this paper, the optimum processing of bromomethyl substituted glycoluril from 1,4-dibromo-2,3- butanedione was studied. The optimum test condition were the follows: molar ratio of bromo-diacetyl to urea being 1:5, the mixture of alcohol and water as solvent, stirring the system for 24h, then adding trifluoroacetic acid 2.5% volume fraction and keeping the reaction last for 48 h, the yield up to 60.8 %. The bromomethyl substituted glycoluril diether was synthesized by bromomethyl substituted glycoluril and paraformaldehyde in hydrobromic acid - ice acetic acid system under 75 ℃. The reaction time was 1h and the yield was 65.5%. The yield of the two compounds mentioned above were increased by 20%-30% compared with the literature. The composition and structure of the compounds were determined by 1HNMR and X ray single-crystal diffraction. |
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