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PCl3- and organometallic-free synthesis of tris(2-picolyl)phosphine oxide from elemental phosphorus and 2-(chloromethyl)pyridine hydrochloride
Tetrahedron Letters ( IF 1.8 ) Pub Date : 2018-01-06 , DOI: 10.1016/j.tetlet.2018.01.021
Svetlana F. Malysheva , Nataliya A. Belogorlova , Vladimir A. Kuimov , Yurii I. Litvintsev , Irina V. Sterkhova , Alexander I. Albanov , Nina K. Gusarova , Boris A. Trofimov

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.



中文翻译:

从元素磷和2-(氯甲基)吡啶盐酸盐合成PCl 3-和无有机金属的三(2-甲基吡啶基)氧化膦合成

在超碱KOH / H 2 O /甲苯/相转移催化剂体系中,由2-(氯甲基)吡啶盐酸盐原位生成的2-picolyl chloride与元素磷在65–95°C下反应3 h,得到三(2-甲基吡啶基)氧化膦,产率为50%。后者的单晶X射线分析表明该叔膦氧化物的一种多晶型物形式。

更新日期:2018-01-06
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