在正相条件下,首次对一系列N-苄氧甲酰基-α-氨基膦酸二苯酯化合物在环糊精类固定相CYCLOBONDI SN和Pirkle型固定相Sumichiral OA 4700上实现了高效液相色谱手性拆分,探索运用定量结构-对映异构体选择性保留关系的方法,将对映异构体的...在正相条件下,首次对一系列N-苄氧甲酰基-α-氨基膦酸二苯酯化合物在环糊精类固定相CYCLOBONDI SN和Pirkle型固定相Sumichiral OA 4700上实现了高效液相色谱手性拆分,探索运用定量结构-对映异构体选择性保留关系的方法,将对映异构体的色谱保留和溶质分子描述参数相关性联系建立定量方程,对比研究了这二种不同类型的手性固定相对该系列有机磷化合物的色谱保留和手性识别机理,结果表明:对该系列化合物而言,Pirkle型手性固定相Sumichiral OA 4700的色谱手性拆分能力明显优于在β-环糊精上衍生引入了额外的与前者类同的Pirkle型不对称中心的环糊精类固定相CYCLOBONDI SN;环糊精类固定相CYCLOBONDI SN在正相色谱条件下,包结机理不起主要作用,其作用方式更接近"Pirkle"型手性固定相;虽然二者具有类同的Pirkle型不对称中心,但是,手性识别机理差异显著,在CYCIOBOND I SN手性固定相上,对N-苄氧甲酰基-α-氨基膦酸二苯酯化合物色谱拆分贡献较大的是其logP和Angle参数相应的相互作用,环糊精提供的不对称性环境对手性识别有重要影响;而SumichiraklOA 4700对该系列化合物的手性识别与locD和TE相应的作用力相关.展开更多
：The crystalline layered and amorphous samples of Zr(HPO4)[O3PCH2N(CH2CO2H)2]· nH2O(n=1,2)(c-or a-ZPPMIDA) and Zr(HPO4)[O3PCH2N(CH2CH2)2O]· nH2O)(n=1,2) (c- or a-ZPMMPA) were prepared with zirconium oxychlo...：The crystalline layered and amorphous samples of Zr(HPO4)[O3PCH2N(CH2CO2H)2]· nH2O(n=1,2)(c-or a-ZPPMIDA) and Zr(HPO4)[O3PCH2N(CH2CH2)2O]· nH2O)(n=1,2) (c- or a-ZPMMPA) were prepared with zirconium oxychloride, sodium dihydrogen phosphate and H2O3PCH2N(CH2CH2)2O(MMPA) or H2O3PCH2N(CH2CO2H)2(PMIDA) in the presence or absence of hydrofluoric acid for the first time.The samples were comparatively characterized by XRD,IR, TG-DTA and elemental analysis. The interlayer spacings of c-ZPPMIDA and c-ZPMMPA were also measured and calculated. XRD results showed that interlayer spacings of c- ZPMMPA and c-ZPPMIDA were 16.055? and 15.384? respectively. The similar structure Zr[(O3PCH2)2NCH2 CO2H]· H2O(ZGDMP) were used to analytically compare with c-ZPMMPA and c-ZPPMIDA. The influences of distribution and rigidity of organic groups on the interlayer spacing were discussed.展开更多
文摘在正相条件下,首次对一系列N-苄氧甲酰基-α-氨基膦酸二苯酯化合物在环糊精类固定相CYCLOBONDI SN和Pirkle型固定相Sumichiral OA 4700上实现了高效液相色谱手性拆分,探索运用定量结构-对映异构体选择性保留关系的方法,将对映异构体的色谱保留和溶质分子描述参数相关性联系建立定量方程,对比研究了这二种不同类型的手性固定相对该系列有机磷化合物的色谱保留和手性识别机理,结果表明:对该系列化合物而言,Pirkle型手性固定相Sumichiral OA 4700的色谱手性拆分能力明显优于在β-环糊精上衍生引入了额外的与前者类同的Pirkle型不对称中心的环糊精类固定相CYCLOBONDI SN;环糊精类固定相CYCLOBONDI SN在正相色谱条件下,包结机理不起主要作用,其作用方式更接近"Pirkle"型手性固定相;虽然二者具有类同的Pirkle型不对称中心,但是,手性识别机理差异显著,在CYCIOBOND I SN手性固定相上,对N-苄氧甲酰基-α-氨基膦酸二苯酯化合物色谱拆分贡献较大的是其logP和Angle参数相应的相互作用,环糊精提供的不对称性环境对手性识别有重要影响;而SumichiraklOA 4700对该系列化合物的手性识别与locD和TE相应的作用力相关.
文摘：The crystalline layered and amorphous samples of Zr(HPO4)[O3PCH2N(CH2CO2H)2]· nH2O(n=1,2)(c-or a-ZPPMIDA) and Zr(HPO4)[O3PCH2N(CH2CH2)2O]· nH2O)(n=1,2) (c- or a-ZPMMPA) were prepared with zirconium oxychloride, sodium dihydrogen phosphate and H2O3PCH2N(CH2CH2)2O(MMPA) or H2O3PCH2N(CH2CO2H)2(PMIDA) in the presence or absence of hydrofluoric acid for the first time.The samples were comparatively characterized by XRD,IR, TG-DTA and elemental analysis. The interlayer spacings of c-ZPPMIDA and c-ZPMMPA were also measured and calculated. XRD results showed that interlayer spacings of c- ZPMMPA and c-ZPPMIDA were 16.055? and 15.384? respectively. The similar structure Zr[(O3PCH2)2NCH2 CO2H]· H2O(ZGDMP) were used to analytically compare with c-ZPMMPA and c-ZPPMIDA. The influences of distribution and rigidity of organic groups on the interlayer spacing were discussed.
