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本文报道双环笼状磷酸酯酰氯(1)与邻氨基酚和邻苯二胺的反应.1与邻氨基酚在硼酸和三乙胺存在下一锅反应可得关环产物1-氧代-4-(2′苯并(口恶)唑基)-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷(2).改变1和邻苯二胺反应的加料顺序可得单酰化产物1-氧代-4-(N-邻苯二胺甲酰基)-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷(5)和双酰化产物1,1′-氧代-4,4′(N,N′-邻苯二胺二甲酰基)-双-(2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷)(4).对产物的 IR,~1H,~(31)P NMR 和 MS 谱进行了研究,并确定了2的晶体和分子结构.结构分析表明,笼状结构 OP(OCH_2)_3C 中基本上不存在应力,仍保持 C_(3v)的对称性,晶体属单斜晶系,空间群 P2_1/c,晶胞参数:a=0.6176(1),b=1.6105(2),c=1.1354(1)nm,β=92.52(1)°,Z=4,最终偏离因子 R=0.056.
In this paper, the reaction of bicyclophosphamide acid chloride (1) with o-aminophenol and o-phenylenediamine was reported.1 One-pot reaction with o-aminophenol in the presence of boric acid and triethylamine gave 1-oxo-4 - (2’benzoxazolyl) -2,6,7-trioxa-1 -phosphabicyclo [2.2.2] octane (2). The charge of 1 and o-phenylenediamine was changed The monoacylation product of 1-oxo-4- (N-o-phenylenecarbamoyl) -2,6,7-trioxa-1-phosphabicyclo [2.2.2] octane (5) And the bisacylation product 1,1’-oxo-4,4 ’(N, N’-o-phenylenediamidoyl) -bis- (2,6,7-trioxa-1-phosphabicyclo [2.2.2] octane) (4). The IR, ~ 1H, ~ (31) P NMR and MS spectra of the product were studied and the crystal and molecular structure of 2 were determined. Structural analysis showed that the cage structure In the OP (OCH_2) _3C, there is almost no stress, and the symmetry of C_ (3v) remains. The crystal belongs to the monoclinic space group P2_1 / c with unit cell parameters of a = 0.6176 (1) and b = 1.6105 2), c = 1.1354 (1) nm, β = 92.52 (1) °, Z = 4, final deviation factor R = 0.056.