Synthesis of 3-Trifluoromethyl-Substituted Benzo[f]chromene Derivatives in a One-Pot Reaction

In the presence of 1,8-diazabicycolo[5.4.0]undec-7-ene (DBU) and concentrated H₂SO₄, 2-naphthol reacted smoothly with α,β-unsaturated trifluoromethyl ketones in CH₂Cl₂ at room temperature, affording the 3-trifluoromethyl-substituted benzo[f]chromene derivatives in good to excellent yields in a one-pot reaction.

[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource: Full experimental and spectral details].     

Phosphate Removal from Aqueous Solution by an Effective Clay Composite Material

Adsorption is an effective treatment process for removing phosphorus and thus controlling eutrophication. In this study, a clay composite material called Al–dolomite–montmorillonite (Al–DM) was prepared and characterized. Al–DM performed well with respect to phosphate removal, with its performance depending on the Al–DM loading, contact time, initial phosphorus concentration and initial solution pH. Adsorption mechanisms were investigated by conducting batch tests on phosphate adsorption using the Al–DM. The adsorption process fitted both the pseudo-second-order kinetics model and the intra-particle diffusion model. The Langmuir, Freundlich and BET models all adequately described the adsorption isotherm data. Thermodynamic studies showed that the adsorption process was endothermic and spontaneous in nature. Al–DM is an effective adsorbent for phosphate removal mainly due to its hierarchical porous structures as shown by characterization with SEM and EDS. Chemical changes occurring before and after adsorption in a water environment indicated that Al–DM had little negative effect on water quality.     

Crosslinked organosiloxane hybrid materials prepared by condensation of silanol and modified silica: Synthesis and characterization

Hybrid materials based on polymethylphenylsiloxane (PMPS) and organic functionalized silica were synthesized via condensation reaction between silanol and alkoxysilyl groups in the presence of quaternary ammonium hydroxide. The structure of prepared materials was investigated by FTIR and NMR, which indicate that the products have incorporated modified silica into the polymer matrix. The prepared hybrid materials show a satisfactory thermal resistance because the initial decomposition of typical product occurred at nearly 100 K higher than that of the pure polymer according to the thermogravimetric analysis (TGA) results. Differential thermogravimetric analysis (DTGA) data confirm that the thermal degradation of prepared hybrid materials comprises of two steps, of which the first one could be controlled by adjusting the content of silica particles and the ratio of surface groups on the particles. The coating films obtained from hybrid products exhibit good thermal mechanical properties. Therefore, the materials are hoped to be used for the application in thermal resistant coating.     

Analysis of operation mode of reflective twisted nematic liquid crystal display devices with rear film compensation

The rear film compensated reflective twisted nematic liquid crystal display device was studied in normally black and normally white operation conditions using a dynamic parameter space method. The electro-optical responses and reflectance spectra were also studied for different operation modes. A comparison was made between rear film and front film compensated reflective twisted nematic liquid crystal displays. We show that high quality normally white or normally black modes can be obtained by placing the fast axis of a quarter wave plate at 45° or 0° to the input director direction. The viewing angle characteristics of the optimum modes were also studied.     

Surface Performance and Cytocompatibility Evaluation of Acrylic Acid-Mediated Carboxymethyl Chitosan Coating on Poly(tetrafluoroethylene-co-hexafluoropropylene)

To improve the biocompatibility of poly(tetrafluoroethylene-co-hexafluoropropylene) (FEP) film, a technique based on Ar plasma pretreatment and UV-induced grafting polymerization was used to immobilize carboxymethyl chitosan (CMCS) on the FEP film surfaces. Initially Ar plasma was used to treat FEP film. Then, plasma treated FEP film was modified via UV-induced grafting polymerization with hydrophilic acrylic acid (AAc) monomer. The following immobilization of CMCS on the FEP-pAAc surface was carried out via an amidation reaction. The change of chemical composition and surface morphology of FEP film were characterized by attenuated total reflectance Fourier transform infrared (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), scanning electronic microscopy (SEM) and atomic force microscopy (AFM). Results of water contact angles measurement showed that the hydrophilicity of the surface has improved significantly after surface modification. Furthermore, methyl thiazolyl tetrazolium (MTT) assay and cell morphology analysis confirmed that mouse fibroblasts (L929 cells) attachment and proliferation were improved remarkably on the modified FEP surface. These results suggest that CMCS were successfully employed to surface engineering FEP film, and enhanced its cell biocompatibility. The approach presented here may be exploited for surface modification of biomaterials.     

Synthesis of 1,4-diarylsubstituted 1,3-diynes through ligand-free copper-catalyzed oxidative decarboxylative homocoupling of aryl propiolic acids

An efficient method of ligand-free Cu-catalyzed oxidative decarboxylative homocoupling of aryl propiolic acids was developed. When CuI was employed as the catalyst and I₂ as the oxidant, the decarboxylative homocoupling reaction for C_sp–C_sp bond formation in DMSO underwent smoothly to afford the corresponding 1,4-disubstituted 1,3-dialkynes in good to excellent yields without any organic ligands. This catalytic system was applicable to aryl propiolic acids bearing different steric, electronic, and functional groups.     

Enantioselective Reduction of Prochiral Ketones with NaBH4/Me2SO4/(S)-Me-CBS

The enantioselective reduction of prochiral ketones with NaBH₄/Me₂SO₄/(S)-Me-CBS is described. Borane is generated in situ via the reaction of NaBH₄ with Me₂SO₄ in tetrahydrofuran, which is as efficient as the commercial one. Such in situ–generated borane reagent was applied to reduce prochiral ketones in the presence of chiral oxazaborolidine catalyst directly. The corresponding chiral secondary alcohols were obtained with excellent enantiomeric excesses (93–99% ee) and good to excellent yield (80–99%).     

Well‐Defined High Molecular Weight Polystyrene with High Rates and High Livingness Synthesized via Two‐Stage RAFT Emulsion Polymerization

A highly living polymer with over 100 kg mol⁻¹ molecular weight is very difficult to achieve by controlled radical polymerization since the unavoidable side reactions of irreversible radical termination and radical chain transfer to monomer reaction become significant. It is reported that over 500 kg mol⁻¹ polystyrene with high livingness and low dispersity could be synthesized by a facile two‐stage reversible addition–fragmentation transfer emulsion polymerization. The monomer conversion reaches 90% within 10 h. High livingness of the product is ascribed to the extremely low initiator concentration and the chain transfer constant for monomer unexpectedly much lower than the well‐accepted values in the conventional radical polymerization. The two‐stage monomer feeding policy much decreases the dispersity of the product.

     

The new synthesis of sulfuryl-bridged triazinane and its selective recognition to SO42−

Research on Chemical Intermediates - A new method has been developed for the synthesis of a cage-like sulfuryl-bridged triazinane molecule HEXS by acidic condensation of a glycoluril analog with...     

Monitoring the kappa number of bleached pulps based on FT-Raman spectroscopy

Cellulose - A new strategy was proposed to determine the Kappa number of bleached Eucalyptus globulus kraft pulps based on FT-Raman spectroscopy. Before modeling, smoothing (Savitzky-Golay),...