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Synthesis of Phosphine Chalcogenides Under Solvent‐Free Conditions Using a Rotary Ball Mill
Author(s) -
Kumar Rajnish,
Kumar Saurabh,
Pandey Madhusudan K.,
Kashid Vitthalrao S.,
Radhakrishna Latchupatula,
Balakrishna Maravanji S.
Publication year - 2018
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201701414
Subject(s) - chemistry , ball mill , phosphine , selenide , atom economy , sulfide , mechanochemistry , grinding , organic chemistry , inorganic chemistry , selenium , chemical engineering , metallurgy , catalysis , materials science , engineering
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 31 P{ 1 H} 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.