A novel supramolecular sodium N,N-piperazinebis(methylenephosphonate) Na 2[(HO 3PCH 2)\5NC 4H 8N(CH 2PO 3H)](H 2O) 8·2H 2O, self-assembled into infinite 1D chains, was synthesized by the reaction of N,N-piperazin...A novel supramolecular sodium N,N-piperazinebis(methylenephosphonate) Na 2[(HO 3PCH 2)\5NC 4H 8N(CH 2PO 3H)](H 2O) 8·2H 2O, self-assembled into infinite 1D chains, was synthesized by the reaction of N,N-piperazine bis(methylenephosphonic acid) with NaOH. Its structure was characterized by single crystal X-ray diffraction, ICP and elemental analysis. The compound crystallizes in triclinic system, space group P1 with a=0.659 06(2) nm, b=0.726 73(2) nm, c= 1.158 25(4) nm, α=79.751(2)°, β=75.833(2)°, γ=74.122(2)°, V=0.513 68(3) nm 3, Z=2, D c=1.611 Mg/m 3, μ=0.331 mm -1, F(000)=264, S=1.098, R 1=0.045 2, wR=0.136 0. In the crystal, edge sharing octahedron Na 2O 10 dimers and tetrahedron PO 3C are assembled to an 1D chain via the bridges of heterocycle. 3D supramolecular framework is self-assembled from 1D chains through H-bonds.展开更多
The crystalline chiral zirconium phosphonates with α, γ-type structure, formulated as Zr(PO 4) 0.6(HPO 4) 0.1(O 3PCH 2NHC 4H 7COO-) 0.55(O 3PCH 2NHC 3H 7COOH) 0.55F 0.55·H 2O(mix-ZrPMP, [α] 25 D=-36°) and...The crystalline chiral zirconium phosphonates with α, γ-type structure, formulated as Zr(PO 4) 0.6(HPO 4) 0.1(O 3PCH 2NHC 4H 7COO-) 0.55(O 3PCH 2NHC 3H 7COOH) 0.55F 0.55·H 2O(mix-ZrPMP, [α] 25 D=-36°) and Zr(PO 4) 0.6(HPO 4) 0.1(O 3PCH 2NHCH 2SC 2H 3COO-) 0.55(O 3PCH 2NHCH 2S-C 2H 3COOH) 0.55F 0.55·2.0H 2O(mix-ZrPMT, [α] 25 D=-39°), were obtained in situ by reaction of N-phosphonomethyl-L-proline(H 3PMP) and N-phosphonomethyl-1,3-thiazolidine-4-carboxylic acid(H 3PMTA) with ZrOCl 2·8H 2O in the presence of HF at 90 ℃, respectively. The heterocycle thiazolidine was integrated onto metal-organic frameworks. Of mix-ZrPMP and mix-ZrPMT, the CO 2H, CO- 2 and NH+ groups are remained in layered structures of mixed-type.展开更多
以4-甲基邻苯二酚为原料,经氧化、酯化两步反应合成产物3,4-二羟基苯甲酸乙酯,并采用IR、1 H NMR和13 C NMR对产物结构进行了表征。通过一系列实验,探讨了催化剂TBAB用量、高锰酸钾用量、反应时间、反应温度对3,4-二羟基苯甲酸产率的影...以4-甲基邻苯二酚为原料,经氧化、酯化两步反应合成产物3,4-二羟基苯甲酸乙酯,并采用IR、1 H NMR和13 C NMR对产物结构进行了表征。通过一系列实验,探讨了催化剂TBAB用量、高锰酸钾用量、反应时间、反应温度对3,4-二羟基苯甲酸产率的影响,以及酯化反应中催化剂TsOH用量、乙醇用量、反应时间和反应温度对3,4-二羟基苯甲酸乙酯产率的影响。在最优合成条件下,3,4-二羟基苯甲酸乙酯的产率可达90.5%。实验证明本合成方法提高了产率,降低了成本,具有较好的工业应用前景。展开更多
文摘A novel supramolecular sodium N,N-piperazinebis(methylenephosphonate) Na 2[(HO 3PCH 2)\5NC 4H 8N(CH 2PO 3H)](H 2O) 8·2H 2O, self-assembled into infinite 1D chains, was synthesized by the reaction of N,N-piperazine bis(methylenephosphonic acid) with NaOH. Its structure was characterized by single crystal X-ray diffraction, ICP and elemental analysis. The compound crystallizes in triclinic system, space group P1 with a=0.659 06(2) nm, b=0.726 73(2) nm, c= 1.158 25(4) nm, α=79.751(2)°, β=75.833(2)°, γ=74.122(2)°, V=0.513 68(3) nm 3, Z=2, D c=1.611 Mg/m 3, μ=0.331 mm -1, F(000)=264, S=1.098, R 1=0.045 2, wR=0.136 0. In the crystal, edge sharing octahedron Na 2O 10 dimers and tetrahedron PO 3C are assembled to an 1D chain via the bridges of heterocycle. 3D supramolecular framework is self-assembled from 1D chains through H-bonds.
文摘The crystalline chiral zirconium phosphonates with α, γ-type structure, formulated as Zr(PO 4) 0.6(HPO 4) 0.1(O 3PCH 2NHC 4H 7COO-) 0.55(O 3PCH 2NHC 3H 7COOH) 0.55F 0.55·H 2O(mix-ZrPMP, [α] 25 D=-36°) and Zr(PO 4) 0.6(HPO 4) 0.1(O 3PCH 2NHCH 2SC 2H 3COO-) 0.55(O 3PCH 2NHCH 2S-C 2H 3COOH) 0.55F 0.55·2.0H 2O(mix-ZrPMT, [α] 25 D=-39°), were obtained in situ by reaction of N-phosphonomethyl-L-proline(H 3PMP) and N-phosphonomethyl-1,3-thiazolidine-4-carboxylic acid(H 3PMTA) with ZrOCl 2·8H 2O in the presence of HF at 90 ℃, respectively. The heterocycle thiazolidine was integrated onto metal-organic frameworks. Of mix-ZrPMP and mix-ZrPMT, the CO 2H, CO- 2 and NH+ groups are remained in layered structures of mixed-type.
文摘以4-甲基邻苯二酚为原料,经氧化、酯化两步反应合成产物3,4-二羟基苯甲酸乙酯,并采用IR、1 H NMR和13 C NMR对产物结构进行了表征。通过一系列实验,探讨了催化剂TBAB用量、高锰酸钾用量、反应时间、反应温度对3,4-二羟基苯甲酸产率的影响,以及酯化反应中催化剂TsOH用量、乙醇用量、反应时间和反应温度对3,4-二羟基苯甲酸乙酯产率的影响。在最优合成条件下,3,4-二羟基苯甲酸乙酯的产率可达90.5%。实验证明本合成方法提高了产率,降低了成本,具有较好的工业应用前景。
