Synthesis and Crystal Structure of 4-Salicylimine-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole JI Bao-Minga

The title compound, 4-salicylimine-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole, was obtained by the condensation reaction of 4-amino-3, 5-bis(2-hydroxyphenyl)-1, 2, 4-triazole with salicylaldehyde in methanol. The crystal structure (C21H16N4O3, Mr = 372.38) belongs to monoclinic system, space group P21/n with a = 10.507(2), b = 16.878(3), c = 11.199(2) ? = 110.86(3), V = 1855.9(6) ?, Z = 4, Dc = 1.333 g/cm3, F(000) = 776, (MoK? = 0.092 mm-1, R = 0.0552 and wR = 0.1095 for 1920 reflections ( I > 2.0(I) ). The analytical results of crystal structure show that there are two different non-covalent interactions in the compound. One is hydrogen bond, and the other p-p stacking interaction. These two types of non-covalent interactions play an important role in the packing of crystal.

HPLC法同时测定大黄药材中8个非蒽醌类成分的含量

目的:建立同时测定大黄药材中8个非蒽醌类成分含量的方法。方法:采用高效液相色谱法。色谱柱为Symmetry C18,流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),流速为1.0mL/min,柱温为30℃,检测波长为280nm,进样量为30μL。结果:没食子酸、儿茶素、表儿茶素、白藜芦醇4′-O-葡萄糖苷、表儿茶素没食子酸酯、白藜芦醇4′-O-β-D(- 6″-O-没食子酰)-葡萄糖苷、番泻苷A、4′-羟基苯基-2-丁酮-4′-O-β-D(- 2″-O-没食子酰-6″-O-对羟基桂皮酰)-葡萄糖苷检测进样量的线性范围分别为6.16~2 464 ng(r=0.999 9)、37.4~14 960 ng(r=0.999 9)、7.635~3 054 ng(r=0.999 7)、7.63~3 052 ng(r=0.999 9)、8.32~3 328 ng(r=0.999 9)、11.5~4 600 ng(r=0.999 9)、16.08~6 432 ng(r=0.999 9)、29.3~11 720 ng(r=0.999 9);定量限分别为3.48、4.30、6.40、4.40、3.39、2.87、8.40、4.95ng,检测限分别为2.32、2.58、2.40、2.64、2.26、1.23、4.20、2.97ng;精密度、稳定性、重复性试验的RSD均小于5%;加样回收率分别为94.32%~100.54%(RSD=2.78%,n=6)、91.15%~99.36%(RSD=3.72%,n=6)、92.16%~98.04%(RSD=2.39%,n=6)、93.41%~100.73%(RSD=3.17%,n=6)、93.89%~98.40%(RSD=1.99%,n=6)、92.61%~101.74%(RSD=3.71%,n=6)、92.66%~103.40%(RSD=3.76%,n=6)、95.45%~102.70%(RSD=3.06%,n=6)。结论:所建方法简便、准确、专属性强,可用于同时测定大黄药材中8个非蒽醌类成分的含量。

Chemical Constituents of Rheum tanguticum Maxim.ex Balf.

Aim To study the chemical constituents of the root and rhizome of Rheum tanguticum Maxim. ex Balf. Methods Chemical constituents were isolated and purified by many chromatographic methods, and their structures were elucidated by MS, NMR, and others. Results Twenty compounds were isolated and their structures were identified as β-sitosterol, chrysophanol, aloe-emodin, physcion, rhein, emodin, etc. Conclusion Among these compounds, 4-(4′-hydroxyphenyl)-2-butanone, 4-(4′-hydroxyphenyl)-2-butanone-4′-O-β-D-(2″-...

糙叶败酱中木脂素成分研究

目的 研究糙叶败酱 (PatriniascabraBge .)中的木脂素类化学成分。方法 应用柱色谱和HPLC法分离纯化 ,通过光谱 (IR ,MS ,1 HNMR ,1 3CNMR ,DEPT ,HMQC和HMBC)鉴定其化学结构。结果和结论 分离并鉴定了 4个木脂素类化合物 ,分别鉴定为 :落叶松脂醇 (1) ,4 [1 乙氧基 1 (4′ 羟基 3′ 甲氧基 )苯基 ]甲基 2 (4 羟基 3 甲氧基 )苯基 3 羟甲基四氢呋喃 (2 ) ,异落叶松树脂酚 (3) ,去甲络石糖苷 (4)。化合物 2为新的木脂素 ,化合物 3,4为首次从该属植物中分得。

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.

长链亲脂性氮氧自由基HPN衍生物的设计合成及对缺氧小鼠存活的影响

目的:设计合成长链取代的2-(4′-羟基苯基)-4,4,5,5-四甲基咪唑烷-1-氧基-3-氧化物(HPN)衍生物,以增强HPN的抗缺氧活性。方法:以乙腈为溶剂、碳酸钾为缚酸剂,60℃反应条件下将HPN分别与6-溴己醇、6-溴己酸乙酯和6-溴己烷进行烷基化反应得到3个长链亲脂性HPN衍生物1、3和5;衍生物1在氢氧化钠甲醇/水体系下经过水解反应得到衍生物2;以二氯甲烷为溶剂,N,N′-二异丙基碳二亚胺为脱水剂,HPN与己酸进行酯化反应,得到衍生物4。采用红外光谱、电子顺磁共振和高分辨质谱表征衍生物1~5的结构,高效液相色谱法检测衍生物的纯度,计算油水分配系数(logP值)评估衍生物的脂溶性,并通过缺氧小鼠常压密闭缺氧实验和急性减压耐受实验考察HPN及衍生物1~5的抗缺氧活性。结果:5个衍生物的结构经红外光谱、电子顺磁共振和高分辨质谱分析确认,产率均在92%以上,纯度均在96%以上。衍生物1~5的logP值分别为2.78、2.00、2.04、2.88和3.10,均高于HPN(0.97);在给药剂量为0.3 mmol/kg时均能显著延长常压密闭缺氧小鼠的生存时间,并将急性减压缺氧小鼠的死亡率分别下降至60%、70%、60%、70%、40%。结论:衍生物1~5的合成方法简便,产率较高,且在剂量较小的情况下,仍然表现出类似或优于HPN的抗缺氧活性,其中衍生物5的活性最佳。

白苞裸蒴化学成分研究

目的研究白苞裸蒴Gymnotheca involucrata全草的化学成分。方法利用反相硅胶柱色谱和反相制备液相色谱等手段进行分离纯化,并通过1H-、13C-NMR等波谱技术进行结构鉴定。结果从白苞裸蒴95%乙醇提取物中分离得到10个化合物,分别鉴定为N-苯甲酰基-2-羟基-2-(4′-羟基苯基)-乙胺(1)、N-苯甲酰基-2-(3′,4′-二羟基苯基)-乙胺(2)、6,9-dihydroxy-4,7-megastigmadien-3-one(3)、对羟基苯乙腈(4)、腺苷(5)、5-hydroxy-3,4-dimethy-5-pentyl-2(5H)-furanone(6)curculonone A(7)、3α-hydroxy-5,6-epoxy-7-megastigmen-9-one(8)、gymnothelignan J(9)、gymnothelignan I(10)。结论所有化合物均为首次从白苞裸蒴中分离得到。

雪松松针正丁醇部位化学成分的研究

目的对雪松Cedrus deodara松针正丁醇部位的化学成分进行研究。方法利用硅胶柱及Sephadex LH-20凝胶色谱柱分离、纯化,并根据理化性质及波谱数据进行结构鉴定。结果从雪松松针正丁醇部位分离得到10个化合物,分别鉴定为1-(4′-羟基-3′-甲氧基苯基)-2-[4″-(3-丙醇基)-2″-甲氧基苯基]-1,3-丙二醇(1)、(7S,8R)-9,9′-二羟基-3,3′-二甲氧基-7,8-二氢苯并呋喃-1′-丙醇基新木脂素-4-O-β-D-葡糖苷(2)、(7R,8R)-3′,9,9′-三羟基-3-甲氧基-7,8-二氢苯并呋喃-1′-丙醇基新木脂素-4-O-α-L-鼠李糖苷(3)、(6R,9R)-6-羟基3-oxo-α-ionol-9-O-β-D-glucopyranoside(4)、(6R,9R)-3-oxo-α-ionol-9-O-β-D-glucopyranoside(5)、莽草酸正丁酯(6)、奎宁酸正丁酯(7)、(6S,9R)-6-hydroxy-3-oxo-α-ionol-9-O-β-D-glucopyranoside(8)、5-p-trans-coumaroylguinic acid(9)、(E)-1-O-对香豆酰基-α-D-吡喃葡萄糖苷(10)。结论化合物1～7为首次从该属植物中分离得到。