(±)-7,8-(2,2-二甲基吡喃)-4′-甲氧基黄烷酮的全合成

以 2 ,4-二羟基苯乙酮为起始原料 ,经过异戊烯基取代、脱氢闭环、羟醛缩合、催化环化等步骤完成了天然产物 7,8-( 2 ,2 -二甲基吡喃 ) -4′-甲氧基黄烷酮 ( 1 )的首次全合成 ,中间体查尔酮 5也是天然产物 .

Crystal and Molecular Structure of 1-Methyl-4-(2-( 3,4-dimethoxyphenyl) vinyl) pyridinium 4-Tolylsulfonate Dihydrate C_(16)H_(18)NO_2^+·C_7H_7SO_3^-·2H_2O

The crystal structure of the title compound C16H18NO2+·C7H7SO3-·2H2O, (C23H29NSO7, Mr=463.53) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system with space group P21/n, a=8.101(1), b=8.958(2), c=33.281(5)?,β= 94.910(1)(, V=2406.3(7)?3, Z=4, Dc=1.279g/cm3, μ=0.176mm-1, F(000)=984, final R=0.0409, and Rw=0.0860 for 4401 independent reflections. The result shows that in the crystal structure of the title compound the planar cations have two configurations with equal occupation ratio and are antiparally packed through π…π interactions. Similar packing energies in A and B are probably the main factor that leads to the disorder structure.

Chiral Phosphine Ligands Derived from Sugars8. Crystal and Molecular Structure of Diphenyl (methyl 4', 6'-O-benzylidene-2'-deoxy-α-D-altropyranoside-2-)phosphine Oxide

The crystal structure of the title compound, C26H27O6P, has been determined by single--crystal X-ray diffraction. The crystal is monoclinic with space groupP21, a=16. 193(l), b=5. 804(1), c=12. 512(2) A, β=93. 187(5)°, V=1174. 13A3, Dc=1. 319 g/cm3, F(000) =492, μ= 13. 52 cm-1, Z= 2, and final R= 0. 042and Rw= 0. 040 for 2349 reflections (I≥3σ(I)). Structure analysis revealed that thepyranose and 4, 6-O-benzylidene ring of the title compound adopts a distorted chair conformation.

Synthesis and Crystal Structure of 1-(1'- t- Butyl-5'-methyl-4-pyrazolyl-carbonyl)- 3,5-dimethyl-1H-yl-pyrazole

The crystal structure of 1-(1-t-butyl-5-methyl-4-pyrazolylcarbonyl)-3,5-dimeth- yl-1H-yl-pyrazole ([C14H20N4O]2, Mr = 520.68) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic, space group P with a = 11.049(4), b = 11.313(4), c = 13.964(5) , ?= 69.085(6), b = 75.962(6), = 62.245(6), V = 1436.7(9) 3, Z = 2, Dc = 1.204 g/cm3, m = 0.079 mm-1, F(000) = 560, R = 0.0790 and wR = 0.1416 for 4729 unique reflections with 2635 observed ones (I > 2(I)). The results indicate that the pyrazole rings display aromaticity. The four pyrazole moieties are approximately coplanar in each case. The dihedral angles between planes 1 and 2, 3 and 4 are 40.99 and 10.77? respectively.

HPLC-MS测定奥美沙坦酯中有关基因毒性杂质

建立一种直接测定奥美沙坦酯中基因毒性杂质5-(4′-溴甲基联苯-2-基)四氮唑和5-(4′-二溴甲基联苯-2-基)四氮唑的液相色谱-质谱联用方法。采用色谱柱AgilentZorbaxEclipsePlusC18(250mm×4.6mm,5μm),以0.1%甲酸水溶液-乙腈为流动相;在电喷雾正离子模式下,对m/z315和m/z395离子进行选择性监测。5-(4′-溴甲基联苯-2-基)四氮唑和5-(4′-二溴甲基联苯-2-基)四氮唑的质量浓度分别在0.0094~0.5610μg/mL和0.0182~0.5475μg/mL范围内与峰面积呈良好线性关系;定量限分别为9.35和18.25ng/mL;检测限分别为3.12和6.08ng/mL;平均回收率分别为96.5%(n=9,RSD=4.8%)和98.0%(n=9,RSD=5.1%)。本法操作简便、专属性好、准确度高,可用于奥美沙坦酯中基因毒性杂质5-(4′-溴甲基联苯-2-基)四氮唑和5-(4′-二溴甲基联苯-2-基)四氮唑的检测。

多联吡啶螯合物反相高效液相色谱法分离测定铜(Ⅱ)、钴(Ⅱ)、汞(Ⅱ)

以三联吡啶衍生物６，６”－二甲基－４＇－苯基－２，２＇：６＇，２”－三联吡啶（ＴＰＹ）作柱前显色剂，于ＡｃｃＱ－Ｔａｇ柱上，用内含２．０×１０～（－６）ｍｏｌ／Ｌ ＴＰＹ和０．６ ｍｏｌ／Ｌ ＮａＡｃ－ＨＡｃ缓冲溶液（ｐＨ＝３．５）的甲醇－水溶液（５５：４５，Ｖ／Ｖ）作流动相，流速为１．０ ｍＬ／ｍｉｎ，并以紫外－可见检测器于３１０ｎｍ处进行检测，开发了一种 ＲＰ－ＨＰＬＣ法同时分离测定铜（Ⅱ）、钴（Ⅱ）、汞（Ⅱ）的方法。该方法简便快速，灵敏度高，对于铜、钴、汞的检测限分别是０．００２０、０．００５５和０．００４０ｍｇ／Ｌ。用于实际样品测定，结果满意。

Synthesis and luminescent properties of ternary complex Eu(UVA)_3Phen in nano-TiO_2

By introducing 2-hydroxy-4-methoxy-benzophenone(UVA) and 1,10-phenanthroline(Phen) as the ligands, the ternary rare earth complex of Eu(UVA)3Phen is synthesized, and it is characterized by elemental analysis, mass spectra(MS) and infrared(IR) and ultraviolet(UV) spectroscopy. Results show that the Eu(III) in complex emits strong red luminescence when it is excited by UV light, and it has higher sensitized luminescent efficiency and longer lifetime. The organic-inorganic thin film of complex Eu(UVA)3Phen doped with nano-Ti O2 is prepared, and the nano-Ti O2 is used in the luminescence layer to change the luminescence property of Eu(UVA)3Phen. It is found that there is an efficient energy transfer process between ligands and metal ions. Moreover, in an indium tin oxide(ITO)/poly(N-vinylcar-bazole)(PVK)/Eu(UVA)3Phen/Al device, Eu3+ can be excited by intramolecular ligand-to-metal energy transfer process. The main peak of emission at 613 nm is attributed to 5D0→7F2 transition of the Eu3+, and this process results in the enhanced red emission.

取代三联吡啶光度法测定钴(Ⅱ)

研究了新显色剂 6 ,6″ 二甲基 4′ 苯基 2 ,2′ :6′ ,2″ 三联吡啶 (TPY)与Co(Ⅱ )的显色反应。结果表明 ,在pH 3 0的NaAc HAc缓冲溶液中 ,该试剂与Co(Ⅱ )发生显色反应 ,形成稳定的绿色络合物 ,其λmax=337 6nm ,表观摩尔吸光系数ε=1 0 3× 10 5L·(mol·cm) -1,Co(Ⅱ )浓度在 0～ 15 μg/ 2 5mL范围内符合比尔定律 ,该方法直接用于维生素B12 中微量钴的测定 ,结果满意。

金星蕨中黄酮类化学成分的研究

目的研究金星蕨Parathelypteris glanduligera中的黄酮类化学成分。方法利用硅胶、C18反相硅胶、Sephadex LH-20凝胶等色谱技术对其提取物进行分离纯化,根据化合物的理化性质和光谱数据进行结构鉴定。结果从金星蕨全草甲醇渗漉浸膏中提取分离得到11个黄酮类化合物,分别鉴定为山柰酚(1)、黄芪苷(2)、三叶豆苷(3)、阿福豆苷(4)、山柰酚-3-O-芸香糖苷(5)、槲皮素(6)、槲皮素-3-O-β-D-吡喃半乳糖苷(7)、芦丁(8)、myriciatrin I(9)、3′-甲基-4′,6′-二羟基-2′-甲氧基-査耳酮(10)、3′,5′-二甲基-4′,6′-二羟基-2′-甲氧基-査耳酮(11)。结论所有化合物均为首次从该植物中分离得到。