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首页> 外文期刊>Zeitschrift fur Kristallographie. New crystal structures >Crystal structure of tetraacetylethylenediamine, C_(10)H_(16)N_2O_4
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Crystal structure of tetraacetylethylenediamine, C_(10)H_(16)N_2O_4

机译：四乙酰基乙二胺C_（10）H_（16）N_2O_4的晶体结构

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摘要

The synthesis was performed by a modified method of [1],, Ethyl-enediamine (5,124 g, 0.084 mol) was added dropwise to a mixture of acetic anhydride (125 ml) and anhydrous sodium acetate (0.5 g) contained in a 250 ml three-neck round-bottom flask equipped with reflux condenser, dropping funnel, thermometer, and magnetic stinei, The temperature was maintained at 298 K by use of an ice bath The total time of addition was 10 min The reaction mixture was then heated at reflux for 20 h and cooled to room temperature. The reaction mixture was then rotary evaporated for 2 h, leaving a thick white sludge Water (50 ml) was added, and then the mixture stirred at room temperature for 1 h in order to hy-drolyze any remaining acetic anhydride. This water solution was then extracted twice with ether (75 ml per extraction) and the combined ether layer was dried (MgSCU), filtered, and concentrated on the rotary evaporator at reduced pressure, leaving 11.49 g (69 %) of the title compound (m.p. 148,2-149 0 °C) IR data are available in the CIF.
机译：通过[1]的改进方法进行合成，将乙二胺（5,124 g，0.084 mol）逐滴加入到250 ml的乙酸酐（125 ml）和无水乙酸钠（0.5 g）的混合物中装有回流冷凝器，滴液漏斗，温度计和磁性甾烷的三颈圆底烧瓶，使用冰浴将温度保持在298K。添加的总时间为10分钟。然后将反应混合物加热回流保持20小时并冷却至室温。然后将反应混合物旋转蒸发2小时，留下浓稠的白色污泥加入水（50ml），然后将混合物在室温搅拌1小时以使任何残留的乙酸酐水解。然后将该水溶液用乙醚萃取两次（每次萃取75毫升），并将合并的乙醚层干燥（MgSCU），过滤，并在旋转蒸发仪上减压浓缩，得到11.49 g（69％）的标题化合物（ mp 148,2-149 0°C）CIF中提供了IR数据。

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