无溶剂合成叔碳羟基膦酸酯及其表征

Solvent-free Synthesis and Characterization of Tertiary Hydroxy Phosphates

发展了一种温和的磷酰化酮而得到标题化合物的方法。在碳酸钾催化无溶剂条件下,芳酮与亚磷酸酯形成羟基膦酸酯,该方法也适合对碱敏感的底物。在分离碱性催化剂(如三乙胺)过程中,常常伴随羟基膦酸酯发生重排反应,生成磷酸酯,磷酸酯影响产物纯度,增加产物分离难度;碳酸钾作为催化剂时,实验中未发现羟基膦酸酯发生重排反应。产物经核磁、红外、质谱等表征。

A benign synthesis method of tertiary hydroxyl phosphonates by hydro phosphonylation of unactivated ketones was developed. In the presence of potassium carbonate,aromatic or heteroaromatic ketones can react with phosphite to form tertiary hydroxy phosphonates under solvent-free and mild conditions. The proposed method was also suitable for base-sensitive ketone. Rearrangement of phosphonate to phosphate was carried out in many strong alkaline mediums,the rearrangement was not found in this work. The structures of products were confirmed by NMR,IR and MS.