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PCl3- and organometallic-free synthesis of tris(2-picolyl)phosphine oxide from elemental phosphorus and 2-(chloromethyl)pyridine hydrochloride
Authors:Svetlana F Malysheva  Nataliya A Belogorlova  Vladimir A Kuimov  Yurii I Litvintsev  Irina V Sterkhova  Alexander I Albanov  Nina K Gusarova  Boris A Trofimov
Institution:A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Science, 1 Favorsky Str., 664033 Irkutsk, Russian Federation
Abstract:In the superbase KOH/H2O/toluene/phase-transfer catalyst system, 2-picolyl chloride, generated in situ from 2-(chloromethyl)pyridine hydrochloride, reacts with elemental phosphorus at 65–95?°C for 3?h to afford tris(2-picolyl)phosphine oxide in 50% yield. Single crystal X-ray analysis of the latter revealed one polymorph form of this tertiary phosphine oxide.
Keywords:Tris(2-picolyl)phosphine oxide  Red phosphorus  Superbase  2-(Chloromethyl)pyridine hydrochloride
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