The mechanochemical technique of ball milling has been applied to the solventless and eco‐friendly synthesis of chalcogenides (sulfide and selenide) of a variety of tertiary and aminophosphines. In most of the cases, the products are obtained in almost quantitative yields with high purity by applying a simple workup procedure without using chromatographic techniques or any other purification methods. The scope of this methodology was explored by using a range of phosphines (mono, di and tetra) to synthesize partial as well as mixed chalcogenides. The use of almost equimolar amounts of starting materials and the absence of any byproducts significantly simplifies the product isolation compared with the standard solution state reactions, thus providing a highly atom economic (100 %) method with an ideal E‐factor (E = 0). The solid‐state reactions were monitored by ³¹P{¹H} NMR spectroscopy. The structures of some of the products are also confirmed by single‐crystal X‐ray analyses. Although most of the reactions were carried out on ca. 100‐mg scale, the scaling up of the reaction did not affect the course of the reaction.

中文翻译：

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使用旋转球磨机在无溶剂条件下合成磷化硫属元素化物

球磨的机械化学技术已应用于多种叔和氨基膦硫属化物（硫化物和硒化物）的无溶剂环保合成。在大多数情况下，通过应用简单的后处理程序而无需使用色谱技术或任何其他纯化方法，就可以以几乎定量的产率获得高纯度的产物。通过使用一定范围的膦（一，二和四膦）合成部分和混合硫族化物来探索这种方法的范围。与标准溶液状态反应相比，几乎等摩尔量的起始原料的使用和不存在任何副产物的存在大大简化了产物的分离，从而提供了一种具有理想E值的高度原子经济性（100％）的方法因子（E = 0）。通过³¹ P { ¹ H} NMR光谱监测固态反应。一些产品的结构也通过单晶X射线分析得到了证实。尽管大多数反应都是在约20℃下进行的。100毫克规模时，反应的放大并没有影响反应的过程。