12H-双苯并[1,3,2]-二氧磷杂八环的合成与波谱分析

Synthesis and Spectral Analysis of 12H-Dibenzo[1,3,2]dioxaphosphocins

通过双 ( 2 羟基 3 ,5 二氯苯基 )甲烷 ( 1)与ROPXCl2 (X =O ,S)的关环反应 ,合成了 6 烃氧基 6 氧 (硫 ) 2 ,4,8,1 0 四氯 1 2H 双苯并 [1 ,3 ,2 ] 二氧磷杂八环 ( 3 ) ,3 (X =O)的收率为 62 %～85 % ,并测试了 3的1HNMR ,13 CNMR ,3 1PNMR以及MS.详细报道了 3的13 CNMR中存在的远程偶合现象 ,并探讨了 3的质谱裂解方式 .

The title compounds 12H-dibenzo[ 1, 3, 2 ] dioxaphosphocins (3) were synthesized by the reaction of 2,2'-methylenebis(2, 4-dichlorophenol) (1) with ROPXCl2 (X = O, S) in high yield (X = 0: 62% - 85%) and characterized by IR, H-1 NMR, P-31 NMR, C-13 NMR and MS spectra. The long-range coupling of phosphorus and carbon in C-13 NMR was reported in detail. The favorable mode of fragmentation of 3 in MS spectrum was also discussed.