【摘要】 通过双(3,5-二氯-2-羟基-苯基)甲烷(1)分别与POCl3或PSCl3在三乙胺存在下关环,再与单烷氧基乙醇钠作用,得到了新化合物5或6;以1与P4S10及三乙胺关环的产物4与烷氧基溴乙烷反应得到了7.测试了5,6和7的1H,13C和31PNMR及MS数据,并讨论了其特征.观察到了磷与C1H(C11H)或C3H(C9H)与P的5JPH偶合常数(约为0.9Hz).在1与POCl3关环产物与单甲氧基乙醇反应的产物中,分离到了一个副产物8并确定了它的化学结构.1与POCl3按3∶2的物质的量比在三乙胺存在下反应,得到收率75%的8.更多还原

【Abstract】 From bis(3,5-dichloro-2-hydrxy-phenyl)methane (1), the new [1,3,2] dioxaphosphocins 5, 6 and 7 were synthesized. 1 reacted with POCl3 or PSCl3 to give cyclic compound 2 or 3, which reacted with monoalkyl-1,2-ethandiol to offer 5 or 6. 7 was prepared by the reaction of 1 with P4S10 in the presence of triethylamine, and then reacted with 2-alkoxyl ethyl bromide. The 1H, 13C and 31P NMR and MS spectra of the new compounds were evaluated and discussed. The coupling 5JPH (about 0.9 Hz) of P and C1H or C3H was observed in the first time. A solid compound 8 was separated from the crude product 5 and its structure was determined. When 1 and POCl3 reacted at the molar ratio of 3∶2, 8 was obtained in yield of 70%.更多还原