新型含氟α-氨基膦酸酯的合成和晶体结构

利用含氟苯基亚胺与亚磷酸酯反应,合成了新型含氟α-氨基膦酸酯,通过元素分析、红外光谱、质谱、核磁共振氢谱对其结构进行了表征.X射线单晶衍射测试结果表明:化合物为三斜晶系,空间群P1,a=1.0178(6)nm,b=1.0354(6)nm,c=2.2534(13)nm,α=77.413(10)°,β=78.340(10)°,y=77.540(10)°,V=2.233(2)nm3,Z=4,Dc=1.289 Mg·m-3,μ=O.175 mm-1,F(000)=904.0,最终偏离因子R=0.0728,wR=0.1724.     

新型含二茂铁的α-氨基膦酸酯的合成及表征

将亚磷酸二乙酯与含有二茂铁席夫碱的化合物反应, 合成了一系列新型的含二茂铁的α-氨基膦酸酯, 所有化合物均经过元素分析, IR, 1H NMR, 31P NMR进行表征. 3h的X射线单晶表明, 3h属三斜晶系, P-1空间群, 晶胞参数a＝0.9728 nm, b＝1.1056 nm, c＝1.3713 nm, α＝108.445(2)°, β＝98.649(2)°, γ＝104.890(2)°, 最终偏差因子R＝0.049, wR＝0.1152.     

N-对三氟甲基苯基-α-氨基烷基膦酸酯的合成、晶体结构及生物活性

采用活性基团拼接法将氟原子引入α-氨基烷基膦酸酯中,合成了一系列含氟芳基α-氨基烷基膦酸酯类新化合物,结构经元素分析,IR,1H NMR及MS确认.对所合成的化合物进行了抑制烟草花叶病毒(TMV)田间生物测试,结果表明,该类化合物具有良好的抑制TMV活性,其中4d化合物在0.0005%浓度下对烟草花叶病毒(TMV)防效达到了67.03%.就此对4d化合物作了单晶培养,并就晶体结构进行了X衍射分析.结构表明4d化合物分子属单斜晶系,空间群P21/c.晶胞参数a=1.1957(5)nm,b=1.0664(5)nm,c=1.5943(7)nm,α=90°,β=97.623(8)°,γ=90°,V=2.0150(15)nm3,Z=4.Dc=1.336 Mg/m3,μ=0.189nm-1,F(000)=840.     

α-羟基取代膦酸酯类化合物的合成研究进展

含磷化合物一直是有机化学研究的热点之一,许多合成药物以及天然产物都含有磷原子。其中,α-羟基取代膦酸酯类化合物是重要的有机合成中间体,其在有机合成中的应用一直受到广泛关注。文章详细综述了α-羟基取代膦酸酯类化合物的合成方法。     

含1,3,4-噻二唑α-氨基膦酸酯的合成及其表征

以硫代氨基脲为前体原料, 合成了两种2位为不同烷硫基的5-氨基-1,3,4噻二唑, 采用“一锅煮”的方法, 与不同的醛及亚磷酸酯合成了一系列含1,3,4-噻二唑的α-氨基磷酸酯, 所得产物均经IR, MS, 1H NMR, 31P NMR和元素分析确证结构.     

新型喹啉酮类膦酸酯衍生物的合成与抗菌活性

根据活性结构拼合原理,设计合成了一系列新型喹啉酮类膦酸酯衍生物,其结构经IR,1H NMR,MS及元素分析确认.采用两倍稀释法测试目标化合物对金黄色葡萄球菌、大肠埃希菌、耐甲氧西林金葡菌、耐喹诺酮金葡菌的抑制活性,结果表明:部分目标化合物对耐药菌的抑制作用略优于对照药诺氟沙星,尤以化合物IIIk最好,对MRSA15#,QRSA7#的最小抑菌浓度(MIC)值分别为6.2,3.1 mg/mL.     

新型含1H-吲唑环的α-氨基膦酸酯的合成及表征

以乙二醇为溶剂,邻氟苯丙酮与水合肼环化生成3-乙基-1-H-吲唑(1),进一步经硝化、还原在吲唑环5位引入氨基得到3-乙基-5-氨基l-H-吲唑(3),化合物3与芳香醛的缩合产物席夫碱4a～4k可与亚磷酸酯5m或5n发生进一步亲核加成制得一系列新型5-氨基-3-乙基-1H-吲唑的α-氨基膦酸酯类衍生物6ma～6mk与6na～6nk,所得新化合物均经1H NMR,13C NMR,31P NMR,IR,MS和HRMS确证结构.     

α-氨基膦酸酯的合成方法研究进展

从Lewis催化剂合成法、非Lewis催化剂合成法、绿色合成法3个方面综述了近年来国内外在α-氨基膦酸酯合成研究领域的最新进展.参考文献33篇.     

新型含磺酰基α-氨基膦酸酯的合成

以N-对甲苯磺酰基乙二胺、取代醛、芳酮及亚磷酸酯为原料,采用“一锅煮”合成了一系列新型的含磺酰基的α-氨基磷酸酯,其结构经1H NMR,13C NMR,31P NMR和元素分析表征.     

水杨醛氨基酸席夫碱类α-氨基膦酸酯的合成及生物活性

利用水杨醛氨基酸席夫碱钾盐与亚磷酸二烷基酯的加成反应,合成了9个新型水溶性α-氨基膦酸酯化合物. 其结构经IR、1H NMR、元素分析等测试技术进行了表征. 结果表明,化合物f的初步生物活性测试显示,其具有良好的杀菌和促进植物生长活性.     

Synthesis,Bioactivity and Crystal Structure Analysis of Diisopropyl[（4-cyanopyrazol-3-ylamino）（2-hydroxyl-phenyl） methyl]phosphonate

The title compound,diisopropyl[(4-cyanopyrazol-3-ylamino)(2-hydroxylphenyl) -methyl] phosphonate was synthesized by the addition reaction of diisopropyl phosphite and N-(4-cyanopyrazole-3-yl) -2-hydroxylphenyl-imine. Its structure was characterized by IR,1H NMR,elemental analysis and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a = 9.1840(13) ,b = 9.2278(13),c = 12.1952(17) ,α = 93.846(2) ,β = 90.947(2) ,γ = 111.289(2) °,V = 959.9(3) 3,Dc = 1.309 g/cm3,Z = 2,μ(MoKa) = 0.173,F(000) = 400,the final R = 0.0414 and wR = 0.1196 for 2985 observed reflections(I > 2σ(I)) . The pyrazole and benzene moieties are approximately coplanar in each case. The dihedral angle between planes 1 and 2 is 82.99°. The crystal structure is stabilized by three intermolecular hydrogen bonds of O(1) -H(1) …O(2) ,N(2) -H(2) …N(3) and N(2) -H(2) …O(1) . Preliminary bioassay indicated that the title compound possessed antiviral activity to some extent.     

Synthesis of Chromonyl-Containing α-Aminophosphonates

A series of novel chromonyl-containing α-aminophosphonates were synthesized by a one-pot reaction from 3-formylchromones, substituted aromatic amines, and dialkylphosphites. Synthesized compounds were characterized by elemental analysis, and ¹H NMR and IR spectroscopy. Single crystal x-ray diffraction data of compound 6e was obtained, and analysis indicates that the crystal belongs to triclinic system with space group P-1, a = 9.4200(4) Å, b = 10.5970(6) Å, c = 12.3506(5) Å, α = 84.178(2)°, β = 73.5830(10)°, γ = 68.2720(10)°. V = 1098.59(9) ų, Z = 2, μ = 0.163 mm^?1, F(000) = 456, R[F²>2σ(F²)] = 0.0835, ωR(F²) = 0.2328.     

两个噻吩并萘并吡喃类化合物的合成及结构表征

以2,7-萘二酚为原料分别经六步反应合成了两个新的角型噻吩并萘并吡喃化合物6和8。两个目标化合物及所有新中间体的结构均经^1HNMR、MS、IR、元素分析充分表征。测定了化合物6的单晶分子结构,其特殊的分子平面刚性和α-吡喃与噻吩部分的活泼双键间的空间结构使之成为更有效的单官能团DNA嵌入剂。     

超声辐射下O,O'-二正丁基-α-(4-三氟甲基苯胺基)-2-氟苯基膦酸酯的合成与晶体结构

采用BF₃•Et₂O催化和45 kHz超声辐射下亚磷酸丁酯与邻氟苯甲醛、对三氟甲基苯胺在78～80 ℃, 无溶剂条件下进行类 Mannich 反应, 0.5 h即可以较高收率获得目标化合物α-氨基膦酸酯(4), 其结构经元素分析, ¹H NMR, IR及MS确认. 对化合物晶体结构进行X衍射分析, 结果表明化合物属单斜晶系, 空间群P2(1)/c, 晶胞参数a＝1.348(4) nm, b＝1.734(4) nm, c＝1.099(3) nm, α＝90°, β＝109.71(4)°, γ＝90°, V＝2.417(11) nm³, Z＝4, D_c＝1.268 g/m³, μ＝0.166 mm^－1, F(000)＝968.     

Synthesis and structural characterization of two cationic dinuclear cymene-ruthenium(II) complexes with thiolato and chloro bridges

Treatment of [(p-cymene)RuCl₂]₂ with HSp-Tol or HSCH₂Ph in the presence of K[PF₆] gave the cationic dinuclear cymene–ruthenium(II) complexes [(p-cymene)₂Ru₂(μ-Cl)(μ-Sp-Tol)₂][PF₆] (1) and [(p-cymene)₂Ru₂(μ-Cl)(μ-SCH₂Ph)₂][PF₆] (2), respectively, which have been characterized by IR, NMR spectroscopies and mass spectrometry along with microanalyses. Their crystal structures were determined by single-crystal X-ray diffraction analyses. The structures of the cationic complexes contain the unusual pseudo-trigonal-bipyramidal Ru₂S₂Cl framework without a ruthenium–ruthenium single bond. The two p-cymene–ruthenium units are held together by two bridging thiolates and one bridging chloride.     

磷系阻燃剂杂环己内磷酸酯衍生物的合成及性能研究

近年来,高分子材料被引燃而导致的火灾事故日益频繁,特别是公共场所的特、重大火灾时有发生,给人民生命财产造成巨大损失。因此,对高分子材料进行阻燃处理,赋予其难燃性和抑烟性,有助于提高其防火安全性和减少火灾损失。在过去相当长时间里,卤系阻燃剂在高分子材料阻燃中发挥着     

Synthesis and structural characterization of 3-thienyl alkyl imides

Five new thiophene imides having the structures C₄H₃SC(O)N(H)C(O)R (where R=Me, Et, Pr, t-Bu, 1-4) and C₄H₃SCH₂C(O)N(H)C(O)CH₃5 have been prepared. Control over the orientation of the carbonyl groups was achieved by the introduction of a bulky group in the terminal position of the side chain, and molecular modeling calculations indicated that the energy difference between the ct and tt conformations is small. The acidity of 1-4 decreases from Me to t-Bu, and, although 1-4 will not undergo oxidative polymerization, the introduction of a single spacer CH₂ group allows 5 to polymerize.     

Synthesis,X-ray Crystallographic Analysis and Bioactivities of α-Aminophosphonates Featuring Pyrazole and Fluorine Moieties

A series of novel -aminophosphonates containing pyrazole and fluorine moieties was designed and synthesized through ultrasonic-assisted condensation and solvent-free addition reactions. Their structures were verified by IR, 1H NMR, 13 C NMR and elemental analysis. The crystal structure of diethyl[(4-cyano-1H-pyrazol-3-ylamino)(3,5-difluorophenyl)methyl]phosphonate(4a, C15H17F2N4O3P) was determined by single-crystal X-ray diffraction. Compound 4a crystallizes in the triclinic system, space group P1 with a = 8.381(3), b = 10.103(5), c = 11.268(3) , = 83.772(19), = 74.726(19), = 70.964(18), V = 869.9(6) 3, Mr = 370.30, Dc = 1.414 g/cm3, Z = 2, F(000) = 384, = 0.200 mm-1, Mo Ka radiation( = 0.71073 ), the final R = 0.0487 and w R = 0.0823 for 1582 observed reflections with I 2(I). X-ray diffraction analysis reveals that there are two planes in 4a, and the dihedral angle is 71.51. Two intermolecular hydrogen bonds and a face-to-face ··· stacking interaction are observed in the crystal structure. The compounds were evaluated for their antifungal, antiviral and antitumor activities, respectively. Among them, 4b, 4c, 4g and 4h exhibit good activities on Sclerotium rolfsii Sacc at 200 μg/m L, while 4b, 4c, 4f and 4g possess good anti-TMV activities at 500 μg/m L. Unfortunately, all of the compounds showed weak antitumor activities.     

Synthesis and crystal structure of ethyl benzimidazole-2-yl phosphonate

When N-cyanoimido-( O,O-diethyl)phosphonyl/S-methyl thiocarbonate (1) was treated with o-phenylenediamine in the presence of Et3N in ethanol,diethyl benzimidazole-2-yl phos-phonate (2) was obtained and hydrolyzed during the recrys-tallization in MeOH/H2O,generating ethyl benzimidazole-2-yl phosphonate (3).Hie crystal structure of compound 3 was determined by X-ray diffraction method.The crystals belong to monoclinic,space group C2/c,a = 1.78408(18) ,6 = 0.83725(9),c= 1.67401(18) nm,β= 118.997(2),V = 2.1870(4) nm3,Z = 8,Dc=1.374 g/cm3,F(000)=944.The final R and wR are 0.0499 and 0.1436,respectively.The mechanism of the above reaction is also discussed.