Quantitative determination of residual 2-(2-chloroethoxy) ethanol (CEE) in quetiapine fumarate by gas chromatogaraphy

A simple and specific gas chromatographic method developed and validated for the determination of 2-(2-chloroethoxy) ethanol in Quetiapine Fumarate. The method is carried out with a flame ionization detector and DB-FFAP capillary column. The linearity was established over a range of 40-150 μg ml-1 and correlation coefficient is more than 0.999.

Solubility of CO_(2) in nonaqueous system of 2-(butylamino)ethanol with 2-butoxyethanol:Experimental data and model representation

Nonaqueous amine-based system is an attractive solution to overcome high-energy-intensive CO_(2) capture process using the conventional aqueous amines.Advanced nonaqueous absorbent of 2-(butylamino)ethanol(BAE)with 2-butoxyethanol(2-BE)has been recently proposed for low-energyconsumption CO_(2) capture.In this work,Henry’s law constants of CO_(2) in the BAE/2-BE blend were obtained by N_(2)O/CO_(2) analogy,and correlated in the temperature range of(283–333)K.Vapor-liquid equilibrium(VLE)data for the BAE+CO_(2)+2-BE system at 65.4%(mass)BAE were also determined in a stirred equilibrium cell at temperatures of(313–393)K and CO_(2) partial pressures up to 275 kPa.A single apparent equilibrium constant KCO_(2);app was proposed for this system and correlated as a function of temperature,carbonated degree of amine and CO_(2) loading.Solubility data were well represented by the modified Kent-Eisenberg model with an average absolute relative deviation(AARD)of 13%.

Quaternary phosphonium polymer-supported dual-ionically bound[Rh(CO)I_(3)]^(2-)catalyst for heterogeneous ethanol carbonylation

A single-Rh-site catalyst(Rh-TPISP)that was ionically-embedded on a P(V)quaternary phosphonium porous polymer was evaluated for heterogeneous ethanol carbonylation.The[Rh(CO)I_(3)]^(2-)unit was proposed to be the active center of Rh-TPISP for the carbonylation reaction based on detailed Rh L3-edge X-ray absorption near edge structure(XANES),X-ray photoelectron spectroscopy(XPS),and Rh extended X-ray absorption fine structure(EXAFS)analyses.As the highlight of this study,Rh-TPISP displayed distinctly higher activity for heterogeneous ethanol carbonylation than the reported catalytic systems in which[Rh(CO)_(2)I_(2)]^(-)is the traditional active center.A TOF of 350 h^(-1)was obtained for the reaction over[Rh(CO)I_(3)]^(2-),with>95%propionyl selectivity at 3.5 MPa and 468 K.No deactivation was detected during a near 1000 h running test.The more electron-rich Rh center was thought to be crucial for explaining the superior activity and selectivity of Rh-TPISP,and the formation of two ionic bonds between[Rh(CO)I_(3)]^(2-)and the cationic P(V)framework([P]^(+))of the polymer was suggested to play a key role in firmly immobilizing the active species to prevent Rh leaching.

Catalytic dechlorination and detoxification of 1-(2-chlorophenyl) ethanol by Pd/Fe

1-(2-chlorophenyl) ethanol (CPE) is of health and environmental concern due to its toxicity and its use as an inter-mediate in pharmaceutical manufacturing. The current work deals with the catalytic reductive dechlorination and detoxification of CPE by Pd/Fe bimetal. CPE was effectively dechlorinated to 1-phenyl ethanol (PE) accompanied by the equivalent release of chloride. The extent of CPE dechlorination increased with temperature,Fe dosage and Pd loading. A decrease in solution pH increased CPE dechlorination,resulting presumably from an increase in hydrogen production. Under the specific conditions of 20 g/L Pd/Fe,0.10% Pd (w/w) and initial pH 5-6,the CPE dechlorination was completed within 145 min. The dechlorination fol-lowed a pseudo-first-order kinetics with an activation energy of 56.7 kJ/mol. The results of toxicity testing showed that CPE was very toxic to Chlorella,whereas PE showed little toxicity. The toxicity of the reaction solution declined gradually and the pro-moting effects on Chlorella intensified consequently with the dechlorination process. Thus,the reductive dechlorination of CPE to PE by Pd/Fe was a detoxification process. It may be used to effectively reduce the toxicological effects of CPE-contaminated wastewater,thereby enhancing the performance of subsequent biological processes in wastewater treatment.

Sensitive and fast response ethanol chemical sensor based on as-grown Gd_2O_3 nanostructures

Well crystalline gadolinium oxide（Gd2O3） nanostructures were grown by annealing the hydrothermally as-prepared nanostructures without using any template. Microscopic studies of Gd2O3 nanostructures were recorded along the [111] direction due to the clearly resolved interplanar distance d（222）-0.31 nm of the cubic crystal structure Gd2O3. Sensing mechanism of Gd2O3 as efficient electron mediator for the detection of ethanol was explored. As-fabricated sensor demonstrated the high-sensitivity of -0.266 μAm/M/cm2 with low detection limit（-52.2 μmol/L） and correlation coefficient（r^2, 0.618）. To the best of our knowledge, this was the first report for the detection of ethanol using as-grown（at 1000 oC） Gd2O3 nanostructures by simple and reliable Ⅰ-Ⅴ technique and rapid assessment of the reaction kinetics（in the order of seconds）. The low cost of the starting reagents and the simplicity of the synthetic route made it a promising chemical sensor for the detection of various toxic analytes, which are not environmentally safe.

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.

Design, Synthesis and Biological Evaluation of 2-（2-Aryl- morpholino-4-yl）ethyl Esters of Indomethacin as Potential Cyclooxygenase-2 （COX-2） Inhibitors

A number of novel 2-（2-arylmorpholino-4-yl）ethyl 1-（4-chlorobenzoyl）-5-methoxy-2-methyl-lH-indol-3- acetate hydrochlorides were synthesized and tested for their cyclooxygenase （COX-1 and COX-2） inhibition prop- erties in vitro. Many of these compounds exhibited moderate to good selective COX-2 inhibition, and subtle struc- tural changes in the substituents on the side chain of the ester moiety altered the inhibitory properties significantly. 2-[2-（4-Butoxyphenyl）morpholino-4-yl]ethyl 1-（4-chlorobenzoyl）-5-methoxy-2-methyl-IH-indol-3-acetate hydro- chloride （If）, showed good selective COX-2 inhibitory activity （Selective index （SI） 182）, which is comparative with celecoxib （SI 214）, a COX-2 inhibitor of diarylpyrazoles. While 2-[2-（2,4-dichloro-5-fluorophenyl）mor- pholino-4-yl]ethyl 1-（4-chlorobenzoyl）-5-methoxy-2-methyl-IH-indol-3-acetate hydrochloride （lg）, showed greater selective COX-2 inhibitory activity （SI 358） than celecoxib. Both compounds were identified as compromising de- rivatives in this class to reduce the side effects generated by nonsteroidal anti-inflammatory drugs （NSAIDs） indo- methacin.

Two New Compounds from Melanosciadum pimpinelloideum H. Boiss

Two new compounds, melanochromone and 2-ethoxyl-2-(4-hydroxyphenyl)ethanol. were isolated from the whole plants of Melanosoiadum pimpinelloideum II. Boiss. The known compounds isolated were 1-(4-hydroxyphenyl)-1.2ethanediol. tymine. cimifugin, umtatin. bergenin. daucosterol and stigmasterol. Their structures were determined on the basis of spectral data.

野核桃叶化学成分研究

目的研究野核桃Juglans cathayensis叶的化学成分。方法使用多种柱色谱技术对野核桃叶95%乙醇提取物进行分离纯化,根据理化常数和波谱数据对化合物的结构进行鉴定。结果共鉴定出21个单体化合物,分别为2-(n-octacosanoxy)ethanol(1)、(+)-galeon(2)、jugcathnin A(3)、2-乙氧基胡桃醌(4)、山柰酚(5)、山柰酚-3-O-吡喃葡萄糖苷(6)、槲皮素-3-O-吡喃葡萄糖苷(7)、6,7-二羟基香豆素(8)、Z-P-coumaryl-hexacosanoate(9)、香草酸(10)、咖啡酸(11)、邻苯二甲酸(12)、二十四烷酸(13)、二十八烷醇(14)、十六烷酸-α-单甘油酯(15)、二十九烷醇(16)、二十五烷醇(17)、硬脂酸(18)、软脂酸(19)、β-谷甾醇(20)、β-胡萝卜苷(21)。结论化合物1为新化合物,化合物2～21均为首次从野核桃叶中分离得到。