有机化学 ›› 2003, Vol. 23 ›› Issue (11): 1271-1276. 上一篇    下一篇

研究论文

12H-双苯并[1,3,2]-二氧磷杂八环的合成与波谱分析

杨代斌;陈万义;李重九   

  1. 中国农业科学院植物保护研究所;中国农业大学应用化学系
  • 发布日期:2003-11-25

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

Yang Daibin;Chen Wanyi;Li Chongjiu   

  1. Institute of Plant Protection, Chinese Academy of Agricultural Science;Department of Applied Chemistry, China Agricultural University
  • Published:2003-11-25

通过双(2-羟基-3,5-二氯苯基)甲烷(1)与ROPXCl_2 (X = O,S)的关环 反应,合成了6-烃氧基-6-氧(硫)-2,4,8,10-四氯-12H-双苯并[1,3,2]-二氧磷杂 八环(3),3(X = 0)的收率为62%-85%,并测试了3的~1H NMR,~(13)C NMR,~ (31)P NMR以及MS。详细报道了3的~(13)C NMR中存在的远程偶合现象,并探讨了3 的质谱裂解方式。

关键词: 氧杂环化合物, 磷杂环化合物, 质子磁共振谱法, 质谱法, C13核磁共振谱法

The title compounds 127/-dibenzo[l,3,2]dioxaphosphocins (3) were synthesized by the reaction of 2,2'-methylenebis(2,4-dichlorophenol) (1) with ROPXC1_2 (X = O, S) in high yield (X = 0: 62% ~85%) and characterized by IR, ~1H NMR, ~(31)P NMR, ~(13)(C NMR and MS spectra. The long-range coupling of phosphoras and carbon in ~(13)C NMR was reported in detail. The favorable mode of fragmentation of 3 in MS spectrum was also discussed.

Key words: OXYGEN HETEROCYCLICS;PHOSPHOROUS HETEROCYCLIC COMPOUNDS;1HNMR, MS;C13NMR

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