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以溴化四正丁铵为催化剂,在相转移催化条件下以KMnO_4氧化环三(邻亚藜芦基)(Cyclotriveratrylene,简称CTV),得到了CTV-5,10-二酮。经~1H-NMR和X-射线衍射法测定,为一近似的“马鞍”形立体结构。此化合物属正交晶系,空间群为D_(2h)~(25)-Pbca。晶胞参数为a=14.301(3),b=16.411(4),c=24.040(4)(?),V=5642.0(?)~3,F(000)=2400(e),Z=8,Dc=1.33g/Cm~3,μ_(MoKa)=1.1cm~(-1)。用SHELXTL直接法解出,以最小二乘修正。 用稀释法合成了1,10-二氧代-2,9-二氮杂-[10](2,6)-吡啶并环蕃和1,10,17,26-四氧代-2,9,18,25-四氮杂[2]邻环[2](2,6)-吡啶并[2]邻环[2](2,6)-吡啶并环蕃。
Using tetra-n-butylammonium bromide as catalyst, CTV-5,10-dione was obtained under the condition of phase transfer catalysis using KMnO 4 as oxidant ring (Cyclotriveratrylene, CTV for short). By ~ 1H-NMR and X-ray diffraction method for the determination of a similar “saddle” -shaped three-dimensional structure. This compound is orthorhombic, space group D_ (2h) ~ (25) -Pbca. The cell parameters are a = 14.301 (3), b = 16.411 (4), c = 24.040 (4) (?), V = 5642.0 , Dc = 1.33g / Cm ~ 3, μ_ (MoKa) = 1.1cm -1. Using SHELXTL direct solution, with least squares correction. 1,10-dioxo-2,9-diaza- [10] (2,6) -pyrido-piperidines and 1,10,17,26-tetraoxo-2,9 Tetraazacyclo [2] ortho [2] (2,6) -pyrido [2] ortho-cyclo [2] (2,6) -pyridocarbacycle.