A novel three-component reaction for the synthesis of new 4-azafluorenone derivatives

Reaction of arylidenemalononitriles, 1,3-indanedione, and mercaptoacetic acid or 4-methylbenzenethiol is successfully carried out using microwave heating. It is an efficient and promising synthetic strategy to build the indenopyridine skeleton.     

Fe3+-H2O2-Rh6G化学发光体系测定水中的邻苯二酚

酚类化合物对于人体及其他生物的毒性较大,邻苯二酚作为一种重要的有机化工原料和中间体,在农业、染料、香料、橡胶、医药、感光材料等领域具有广泛的应用。因此监测废水中邻苯二酚的含量是控制水环境质量的一个重要指标。目前测定邻苯二酚的方法主要有光度法[1,2],原子吸收法[     

MODIFICATION OF TRANSITION METAL CATIONS TO POLYMER-STABILIZED PLATINUM COLLOIDAL CLUSTERS IN ENANTIOSELECTIVE HYDROGENATION OF METHYL PYRUVATE

Modification of transition metal cations to polymer-stabilized Pt colloidal clusters modified with cinchonidine was studied in enantioselective hydrogenation of methyl pyruvate. Compared to the enantiomeric excess (e.e.) value (71.4%) obtained without the presence of metal cations, obvious e.e. enhancement (up to 82.5%) was resulted from the addition of Zn^2 but with a certain decrease in activity. The reaction parameters in the presence of Zn^2 were also studied. It was found that the Pt colloidal catalysts in the presence of metal cations performed very differently from that in the absence of metal cations.     

A vacuum ultraviolet photoionization mass spectrometric study of acetone

The photoionization and dissociative photoionization of acetone have been studied at the photon energy range of 8-20 eV. Photoionization efficiency spectra for ions CH3COCH3+, CH3+, C2H3+, C3H3+, C3H5+, CH(2-)CO+, CH3CO+, C3H4O+, and CH3COCH2+ have been measured. In addition, the energetics of the dissociative photoionization has been examined by ab initio Gaussian-3 (G3) calculations. The computational results are useful in establishing the dissociation channels near the ionization thresholds. With the help of G3 results, the dissociation channels for the formation of the fragment ions CH3CO+, CH2CO+, CH3+, C3H3+, and CH3COCH2+ have been established. The G3 results are in fair to excellent agreement with the experimental data.     

One-carbon homologation of carboxylic acids via BtCH(2)TMS: a safe alternative to the Arndt--Eistert reaction

Carboxylic acids are converted into the corresponding homologated acids or esters, using easily available 1-(trimethylsilylmethyl)benzotriazole (1) as a one-carbon synthon. The effectiveness of the reaction has been investigated on six aryl and seven alkyl carboxylic acids.     

Orthogonal, convergent syntheses of dendrimers based on melamine with one or two unique surface sites for manipulation

An orthogonal, convergent route for the introduction of substoichiometric numbers of latent surface sites into dendrimers based on melamine is used to prepare targets that display one or two Boc-protected amines on the periphery. Asymmetry is the result of the stepwise incorporation of functionalized and unfunctionalized dendrons onto the triazine cores, a highly selective process due to the different reactivities of the substituted triazines. The routes to the dendrons rely on iterative reactions of the growing dendrons with triazine cores and diamine linkers. p-Aminobenzylamine is used as a linking group to avoid functional group interconversions or protecting group manipulations. Addition of the benzylamine group to the monochlorotriazine of the dendron proceeds cleanly leaving a less reactive aniline for subsequent reaction with trichlorotriazine. The routes to these targets proceed in 5 or 6 linear steps (11 or 12 total steps) in 40% overall yield. The unique surface sites can be deprotected and subjected to additional chemistries. Reaction of the monofunctionalized dendrimer with trichlorotriazine yields the desired dimer, a molecule whose increased size is evident from light scattering and tapping mode atomic force microscopy, and corroborated with computation.     

Regioselective synthesis of polysubstituted pyrazoles and isoxazoles

A regioselective synthesis has been developed for the preparation of unsymmetrical 1,3,5-triaryl-4-alkylpyrazolines and -pyrazoles by treatment of alpha-benzotriazolyl-alpha,beta-unsaturated ketones with monosubstituted hydrazines followed by alkylation at the 4-position of the pyrazoline ring. Reaction of alpha-benzotriazolyl-alpha,beta-unsaturated ketones with hydroxylamine gives 3,5-disubstituted isoxazoles regioselectively.     

Analysis of combinatorial chemistry samples by micellar electrokinetic chromatography

A micellar electrokinetic chromatography (MEKC) method has been developed that can evaluate the purity of samples generated in combinatorial chemistry libraries. This method uses an open tube capillary (27 cm x 50 microm) along with a run buffer composed of sodium dodecyl sulfate (SDS), hydroxypropyl-beta-cyclodextrin, and sodium tetraborate coupled with UV detection. Neutral compounds and compounds that were insoluble in aqueous buffers could be analyzed under these conditions in approximately 3 min. The concentration of SDS and the concentration of hydroxypropyl-beta-cyclodextrin effected the separation. The affect on selectivity resulting from the addition of an organic modifier to the run buffer was examined. The low background absorbency of the run buffer made for easy detection of compounds that absorbed at low UV wavelengths. The quick analysis time made this suitable for analysis of combinatorial chemistry samples.     

Analysis of acyclovir by high performance capillary electrophoresis with on-column amperometric detection

The separation of acyclovir (ACV) by high performance capillary electrophoresis (HPCE) with on-column amperometric detection using alpha-amino-5-mercapto-3,4-dithiazole (AMD) as internal standard is described. The calibration line was linear in the range of 0.5-20 mg/L of ACV. The detection limit was 0.15 mg/L of ACV. Its recovery ranged from 98 to 101% with relative standard deviations (RSDs) from 1.9 to 3.2% (n = 5). This method was successfully used for determining ACV in some pharmaceuticals and human urine. Comparable results with HPCE with ultraviolet (UV) detection and amperometric detection were obtained.