4-氯-3',4'-二甲氧基二苯甲酮合成工艺研究

以邻二甲氧基苯和对氯苯甲酰氯为原料,无水三氯化铝为催化剂,二氯乙烷为溶剂,合成了4-氯-3',4'-二甲氧基二苯甲酮,经洗涤、蒸馏、重结晶,得到了高纯度产品。研究了反应物投料比、催化剂量、反应时间、溶剂的量、反应温度、重结晶溶剂量等对产品收率和含量的影响。

Oxidation of 4-chloro-3-methylphenol using zeolite Y-encapsulated iron(Ⅲ)-,nickel(Ⅱ)-,and copper(Ⅱ)-N,N'-disalicylidene-1,2-phenylenediamine complexes

The degradation of 4-chloro-3-methylphenol（PCMC）using zeolite-encapsulated iron（III）,nickel（II）,and copper（II）complexes of N,N’-disalicylidene-1,2-phenylenediamine as catalysts,in a heterogeneous Fenton-like advanced oxidation process,was studied.The physicochemical properties of the catalysts were determined using powder X-ray diffraction,thermogravimetric analysis,Brunauer–Emmett–Teller surface area analysis,Fourier-transform infrared spectroscopy,elemental analysis,and scanning electron microscopy.The effects of four factors,namely initial H2O2 concentration,catalyst dosage,temperature,and pH,on the degradation of a model organic pollutant were determined.The results show that at low acidic pH,almost complete removal of PCMC was achieved with the iron（III）,nickel（II）,and copper（II）catalysts after 120 min under the optimum reaction conditions：catalyst dosage 0.1 g,H2O2 concentration 75 mmol/L,initial PCMC concentration 0.35mmol/L,and 50 °C.The reusability of the prepared catalysts in PCMC degradation was also studied and a possible catalyst deactivation mechanism is proposed.The possible intermediate products,degradation pathway,and kinetics of PCMC oxidation were also studied.

Molecular Structural and Properties of 3-chloro-4 (dichloromethyl)-5-hydroxy-2[5H]-furanone (MX)

3 - chloro - 4 (dichloromethyl) - 5 - hydroxy - 2 [5H] - furanone (MX) formed during chlorination of water containing natural organic substances, is a very potent bacterial mutgen. Molecular mechanics calculations to evaluate the conformation of structure, and to determine structure relationship properties are put forward. The investigations allow the correlation of molecular structures of MX with its properties, such as mass,partial charges, steric energy, frontier molecular orbital. The VRML molecular models have been investigated using Virtual Reality software. The spectral simulation of MX is illustrated. The principal aim is to develop an efficient method which control of MX.

Synthesis and Crystal Structure of 4-(2- Chlorophenyl)-5-cyano-3-methyl-6-oxo-1- phenyl-4,5,6,7-tetrahydropyrazolo[3,4-b] Pyridine under Microwave Irradiation

The title compound (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.8192(19), b = 15.976(3), c = 13.094(3) ? = 103.074(4), V = 1797.1(7) ?, Z = 4, Dc = 1.341 g/cm3, = 0.229 mm-1, F(000) = 752, R = 0.0632 and wR = 0.1278. X-ray analysis reveals that the pyridine ring adopts an envelope conformation. The dihedral angle between the pyrazole and pyridine planes is 2.19, and inter- molecular hydrogen bonds are also observed in the molecule.

Effect of 2-amino-2-[2-(4-octylphenyl) ethyl] propane- 1,3-diol hydrochloride (FTY 720) on immune liver injury in mice

AIM: To investigate the protective effect against two immune liver injury models in mice by 2-amino-2-[2-(4-octylphenyl) ethyl] propane-l,3-diol hydrochloride and its possible mechanisms in Con A-induced liver damage. METHODS: Liver tissue or hepatocyte injury was monitored biochemically by measuring alanine aminotransferase (sALT) and aspartate aminotransferase (sAST) activity. Hematoxylin & eosin (HE) staining was used for histopathological examination. To evaluate the role of IFN-γ and IL-4 in the liver injury, serum levels of IFN-γ and IL-4 were determined using commercially available ELISA kit at 12 h after Con A challenge. We also determined FTY 720-induced spleen cell apoptosis by flow cytometry analysis or spleen cell proliferation test. RESULTS: Different doses of FTY 720 treatment dramatically reduced circulating markers of hepatocyte injury in two kinds of immunological liver injury models. FTY 720 dramatically reduced the elevated serum IFN-γ and IL-4 levels after Con A injection. Effect of spleen cell supernatants treated with Con A or FTY 720 on hepatocytes showed that ALT activities in cultured hepatocyte supernatants in Con A treatment group increased markedly and FTY 720 could reduce this elevated ALT activities in FTY 720 treatment group. FTY 720 dose-dependently increased the percentage of apoptotic cells in T cells and inhibited splenocyte proliferation induced by Con A. CONCLUSION: Pretreatment with FTY 720 was shown to produce protective effect on the immune liver injury in mice. The possible mechanism of FTY 720 on Con A-induced liver damage is that it could inhibit lymphocyte proliferation and induce lymphocyte apoptosis, resulting in the reduction of IL-4 or IFN-γ release, and subsequently protecting liver from being damaged by Con A.

Novel Fluorescent Dyes Based on Coumarin System

Seven novel fluorescent coumarin derivatives were synthesized from 7-diethylamino-4-chloro-3-formyl-coumarin. The spectra of absorption, excitation and emission were dependent not only on the structures and also on the concentration of dyes. The PPP-MO predictions can only be consistent with the spectra in dilute solutions.