Crystal Structure and ESIPT Phenomena of Anionic 2H-Phenanthro[9,10-c]pyrazol-11-ols

Using 4?-methoxy-5-hydroxyisoflavone and 4?,5-dihydroxy-7-methoxyisoflavone as leding compounds,6-methoxy-2 H-phenanthro[9,10-c]pyrazol-11-ol(1 a) and 9-methoxy-2 Hphenanthro [9,10-c]pyrazol-6,11-diol(1 b) were synthesized by two dehydration processes in the EtOH solution.They were characterized by IR,~1H NMR and ~(13)C NMR.The black prism crystal of 1 a was grown by the slow solvent evaporation technique from 40:1(v/v) CHCl_3/MeOH,and it was determined by single-crystal X-ray diffraction.In the crystal structure,1 a was stabilized by intramolecular(O–H···N) and intermolecular(N–H···O,O–H···O,π···π,C–H···π) interactions.In addition,the fluorescence properties of 1 a and 1 b in the base and neutral media revealed that they possessed excited state intramolecular proton transfer phenomena(ESIPT).     

Synthesis,Crystal Structure and Antitumor Activity of 4-(5-(2,6-Difluorophenyl)-1,3,4-oxadiazol-2-ylthio)-2-(trifluoromethyl)thieno[2,3-d]pyrimidine

The title compound 4-(5-(2,6-difluorophenyl)-1,3,4-oxadiazol-2-ylthio)-2-(trifluoromethyl)thieno[2,3-d]pyrimidine(C_(15)H_5F_5N_4OS_2, Mr = 416.35) was designed and synthesized as antitumor agent, and its structure was determined by ~1H NMR, ~(13)C NMR, MS, elemental analysis and single-crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P2_1/c with a = 9.904(2), b = 10.057(2), c = 16.595(3) ?, β = 100.000(3)°, V = 1627.9(6) ?~3, Z = 4, F(000) = 832, D_c = 1.699 g/cm~3, μ = 0.395 mm~(-1), R = 0.0468 and wR = 0.1255 for 4726 independent reflections(R_(int) = 0.0336) and 2847 observed ones(I 2σ(I)). The in vitro antitumor activity of the title compound was preliminarily evaluated by the standard MTT assay.     

双功能复合材料g-C3N4/CdS/Ni催化光解水产氢和5-羟甲基糠醛氧化性能

采用高温煅烧法、 原位生长法和光还原法分三步制备出双功能复合光催化剂g-C₃N₄/CdS/Ni. 材料中CdS的引入可以增强光生电子和空穴的分离效率, Ni可以进一步提高光致产氢速率. 在以三乙醇胺(TEOA)为电子给体的水溶液中对所制备的材料进行了催化产氢性能测试, 并对材料中CdS的含量进行了优化. 结果表明, 25% (质量分数)CdS负载量的复合材料催化产氢性能最佳, 其催化产氢速率为4134.5 μmol·g^-1·h^-1, 是 g-C₃N₄/Ni催化产氢速率的115倍. 且Ni是一种良好的质子催化剂. 在此基础上, 以5-羟甲基糠醛(HMF)替代TEOA作为体系的电子给体, 其可以被选择性地催化氧化为增值化学品2, 5-二甲酰基呋喃(DFF). 当体系中HMF的转化率为82.3%, DFF的选择性为69.4%时, DFF的产率(57.2%)达到最高, 体系中H₂的产量为 51.8 μmol/g. g-C₃N₄/CdS/Ni复合材料可以在同一体系中进行催化光致产氢和HMF的选择性氧化.