有机化学 ›› 1993, Vol. 13 ›› Issue (5): 527-532. 上一篇    下一篇

研究论文

1-氧代-1-磷杂-2, 6, 7-三氧杂双环[2.2.2]-4-含硫取代基辛烷 的合成

李玉桂;包建春;李建敏   

  1. 南开大学元素有机化学研究所.天津(300071)
  • 发布日期:1993-10-25

Synthesis of 1-oxo-1-phospha-2, 6, 7-trioxabicyclo[2.2.2]-4-sulphur- containing substituted group octane

Li Yugui;Bao Jianchun;Li Jianmin   

  1. Nankai Univ, Elementoorgan Chem Lab.Tianjin(300071)
  • Published:1993-10-25

本文利用中间体1-氧代-1-磷杂2,6,7-三氧杂双环[2.2.2]-4-羟甲基辛烷(1)和1-氧代-1-磷杂-2,6,7-三氧杂双环[2.2.2]-4-氯甲酰基辛烷(3)分别与RSH或取代硫醇按步骤反应得到了相应的4-亚甲基硫醚(5a~f)、4-亚甲基亚砜(6a~f)、4-(氯代乙硫基)甲酰基(7)及4-(β-烷硫基)-α-硫代酯基(8a~i)的双环笼状磷酸酯新衍生物共22个。所有的化合物经元素分析、IR和^1HNMR得到了证实。

关键词: NMR, 亚砜, 农药, 硫醚, 合成, 元素分析, 硫醇, 双环笼状磷酸酯

In this paper, a new simple method was used in the preparation of 1- oxo-1-phospha-2, 6, 7-trioxabicyclo[2.2.2]-4-chloromethyl octane (4), and new derivatives of bicyclic phosphate (5a~ f, 7, 8a~ i), which are 4-methylene sulfide, 4-chloroethanethioyl carbony, 4-(β - thioalkyl)-α-thioic ester, respectively, were synthesized by the reaction of (4) or 1-oxo-1-phospha-2, 6, 7-trioxabicyclo[2.2.2]-4- chlorocarbonyl octane (3) with mercaptans. The corresponding sulfoxides (6a~f) were also obtained by further oxidation of 5a~f. All the compounds were confirmed by elemental analysis, IR and ^1H NMR.

Key words: SYNTHESIS, PESTICIDES, ELEMENTAL ANALYSIS, MERCAPTAN, SULFOXIDE, SULFUR ETHER, NMR

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