Single-crystal Cultivation and Structure Analysis of Unstable 1-Azido-2-chloro-4-nitrobenzene

The 1-azido-2-chloro-4-nitrobenzene was prepared by nucleophilic substitution between 2-chloro-4-nitro-1-(trifluoromethylsulfinyl)benzene and sodium azide, and its structure was characterized by NMR spectrum and X-ray single-crystal diffraction. It crystallizes in the monoclinic system, space group P21/n, Z = 8 and Mr = 198.57. A cultivation process of the single crystal of unstable aryl azide was provided. The group of trifluoromethyl sulfinyl was found for the first time to be a new excellent leaving group of aromatic nucleophilic substitution reactions.

Protective Effect of Vitamin E on Liver Damage Induced by 2-Chloro-1, 3-butadiene

The present study was performed to determine the influence of lipid peroxidation and perturbance of Ca2+ homeostasis on liver damage induced by 2-chloro-1, 3-butadiene (CBD) and the protective effects of vitamin E in Wistar rats. Animals were given intraperitoneally different doses (8,40 or 200 mg·kg-1 daily) of CBD for 21 days, and the following dose-dependent events were observed: liver damage, significant increase in liver lipid peroxides, and decreases in activities of erythrocytic glutathione peroxidase (GSH-Px) and superoxide dismutase (SOD). The pretreatment of rats with vitamin E (po 150 mg·kg-1) before administering CBD (iP 60 mg·kg-1 ) daily for 21 days prevented the following CBD-induced changes, the increase in serum cholylglycine (CG), hepatic LP, hepatic mitochondrion LP, hepatic oxidized glutathione (GSSG) (while the significant increase of reduced glutathione (GSH) was not affected) and the decrease in activities of erythrocytic SOD and hepatic mitochondrial calcium sequestration. These results suggest that lipid peroxidation and perturbance of Ca2+ homeostasis appear to contribute to the hepatotoxicity of CBD, and vitamin E might prevent the liver damage induced by CBD. The decrease in activities of GSH-Px and SOD in erythrocytes might be used as biomarkers for adverse effects of CBD on defense system against lipid peroxidation.

Et_3NHCl-AlCl_3 Ionic Liquids as Catalyst for Alkylation of Toluene with 2-Chloro-2-methylpropane

Alkylation of toluene With 2-chloro-2-methylpropane （t-Bu-C1） to synthesize para-tert-butyltoluene （PTBT） was carded out in the presence of triethylamine hydrochloride-aluminum chloride ionic liquids used as the catalyst. The ionic liquids were prepared with different molar ratios of Et3NHC1 to A1CI3, and the effect of the molar ratio between A1C13 and Et3NHC1, the reaction time, the reaction temperature, the ionic liquid dosage, as well as the molar ratio of toluene to chloro- 2-methylpropane on the alkylation reaction of toluene with chloro-2-methyl-propane was investigated. The test results showed that the acidic ionic liquids prepared with Et3NHC1 and A1C13 had good activity and selectivity for the alkylation reaction of toluene with alkyl chloride to produce PTBT. The optimal reaction conditions were specified at an A1C13 to Et3N- HCI ratio of 1.6, a reaction temperature of 20 ℃, a mass fraction of toluene to ionic liquid of 10%, and a chloro-2-methyl- propane to toluene molar ratio of 0.5. Under the suitable reaction conditions, a 98% conversion of chloro-2-methylpropane and an 82.5% selectivity of PTBT were obtained. Ionic liquids could be reused 5 times with its catalytic activity unchanged, and the regenerated ionic liquids can be recycled.

Coupling Reaction of 4-Chloro-7-H-Pyrrolo[2,3-d]Pyrimidine with 2,3,5-Tri-O-Acetyl-b-D-Ribofuranosyl Chloride

Coupling reaction of 4-chloro-7-H-pyrrolo[2,3-d]pyrimidine with 2,3,5-tri-O-acetyl -β-D-ribofuranosyl chloride under the basic condition was investigated. An abnormal coupling reaction, in which the heterocyclic base attacked at the carbon of 1,2-O-methylidene moiety instead of anomeric carbon of ribose was observed and the structure of products 5a, 5b were identified by NMR and X-Ray diffraction.

(Z)-N-(3-(2-Chloro-4-nitrophenyl)-4-methylthiazol-2(3H)-ylidene) Pivalamide: Synthesis and Crystal Structure

Synthesis of the title compound was carried out by base-catalyzed cyclization of 1-pivaloyl-3-(2-chloro-4-nitrophenyl) thiourea with α-bromoacetone produced in situ. The structure was confirmed by the spectroscopic and elemental analysis and single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1 with unit cell dime sions a = 8.7137(10), b = 10.2010(14), c = 10.6593(13), α = 62.671(9), β = 82.701(10), γ = 79.762(10), V = 827.21(8) ?3, Z = 2.

Synthesis, Crystal Structure, Thermal Behavior and Photoluminescent Property of Complex [Zn(L)(SO_4)]·0.5H_2O

Complex [Zn（L）（SO4）]0.5H20 （L = 2-（2-chloro-6-fluorophenyl）-lH-imidazo[4,5- J][1,10]phenanthroline） has been synthesized under hydrothermal conditions. The compound was characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 9.9916（7）, b = 12.3834（9）, c = 29.259（2） A, fl = 97.7720（10）°, V = 3587.0（4） A^3, Z = 2, C76H41CI4F4NI60952Zn2, Mr = 1734.91, Dc = 1.606 g/cm^3, F（000） = 1754, p（MoKa） = 0.959 mm-1, R = 0.0492 and wR = 0.1385. The asymmetric unit of 1 contains one Zn（lI） atom, two L ligands, one sulfate anion and half a water molecule. Each Zn（lI） atom is five-coordinated by four nitrogen atoms from two different L ligands and one sulfate oxygen atom in a tetragonal pyramidal coordination environment. The N-H＇＂O hydrogen bonds link the discrete structure of 1 into a 2D supramolecular architecture. The photoluminescent property of 1 has also been studied in the solid state at room temperature.

Synthesis of 2-deoxy-2-chloro-1-amino sugars and evaluation of their cytotoxicity against cancer cells

Using the potent anticancer agent 2-deoxy-2-chloro-1-amino sugar as a lead compound, its analogs were prepared in 6 steps starting from D-glucal. The key step was the synthesis of 2-chloro-1-acetamido sugars using （COCl） 2-AgNO 3-CH 3 CN system in high yields. 2-Deoxy-2-chloro-1-amino sugars were obtained by treating the corresponding acetamido sugars with HCl in MeOH. All the compounds, including the reference compound, displayed almost no cytotoxic activity to the selected cancer cell lines.

Preparation of(R)-2-chloro-1-(m-chlorophenyl)ethanol by Lipozyme TL IM-catalyzed second resolution

（R）-2-Chloro-l-（m-chlorophenyl）ethanol,a precursor of（R）-3-chlorostyrene oxide which is the key chiral intermediate for the preparation of severalβ3-adrenergic receptor agonists was prepared in 40%yield and 99%ee by the Lipozyme TL IM-catalyzed second resolution of the corresponding racemate in the presence of vinyl acetate.

Kinetic Resolution of 2-Chloro-1-（3,4-dichlorophenyl）ethanol by Lipase-Catalyzed Transesterification

Kinetic resolution of racemic 2-chloro-1-（3,4-dichlorophenyl）ethanol was performed by free Alcaligene sp. lipase-catalyzed irreversible transesterification affording the （R）-isomer with ≥95% ee and the （S）-isomer with ≥90% ee. The activity of lipase Alcaligene sp. strongly depends on the basicity of the reaction system, and an organic base such as triethylamine can enhance the activity of the lipase and enantioselectivity markedly.

An approach to synthesis of(Z)-2-chloro-1,3-diarylpropen-1-ones by Vilsmeier reagent(bis-(trichloromethyl)carbonate/DMF)

A series of（Z）-2-chloro-1,3-diarylpropen-1-ones were unexpectedly synthesized in moderate yields by treatment of easily available 2,3-epoxy-1,3-diarylpropan-1-ones with Vilsmeier reagent,which was derived from bis（trichloromethyl） carbonate（BTC, triphosgene） and DMF.A possible mechanism was also proposed,where sequential ring-opening,halogenation and elimination reactions were involved.

Mild and Efficient Synthesis of 1-（6-Chloroquinoxalin-2-yl）-2- [4-（trifluoromethyl）-2,6-dinitrophenyl] Hydrazine Derivatives by Microwave Irradiation

Some 1-（6-chloroquinoxalin-2-yl）-2-[4-（trifluoromethyl）-2,6-dinitrophenyl] hydrazine derivatives have been synthesized via both conventional and microwave assisted organic synthesis（MAOS） methods. The MAOS method is more effective on synthesizing these compounds than the conventional method in regard to the higher chemical yields of products（76%-98%） and the shorter reaction time（1-15 min）.