LiBF4: a mild and novel reagent for the OH insertion reactions of α-diazoketones

Lithium tetrafluoroborate (10 mol%) is found to catalyze efficiently the OH insertion reactions of α-diazoketones with various alcohols including benzylic, allylic, propargylic and cyclopropyl carbinols to produce the corresponding α-alkoxy ketones in excellent yields with high selectivity. A solution of 10 mol% of LiBF₄ in acetonitrile provides a convenient reaction medium to carry out the OH insertion reactions under mild and neutral conditions.     

Co-catalyzed reductive cyclization of azido and cyano substituted α,β-unsaturated esters with NaBH4: enantioselective synthesis of (R)-baclofen and (R)-rolipram

Sodium borohydride in combination with a catalytic amount of CoCl₂ has been found to be an excellent catalytic system in reductive cyclizations of suitably substituted azido and cyano groups of α,β-unsaturated esters to afford γ and δ-lactams in high yields. The process has been demonstrated for the enantioselective synthesis of (R)-baclofen, (R)-rolipram, and (R)-4-fluorophenylpiperidinone, a key intermediate for (−)-paroxetine.     

Sodium bromide catalysed one-pot synthesis of tetrahydrobenzo[b]pyrans via a three-component cyclocondensation under microwave irradiation and solvent free conditions

Sodium bromide catalysed three-component cyclocondensation of aryl aldehydes, alkyl nitriles and dimedone proceeds under microwave irradiation in solvent free conditions to give highly functionalised tetrahydrobenzo[b]pyrans in excellent yields.     

Facile polyethylene glycol (PEG-400) promoted synthesis of β-ketosulfones

An efficient and convenient synthesis of β-ketosulfones is described. Reaction of an α-haloketone with sodium alkyl/aryl sulphinate yields the corresponding β-ketosulfone promoted by polyethylene glycol (PEG-400) as an efficient reaction medium.     

Physicochemical study of ovalbumin in the presence of sodium dodecyl sulphate in aqueous media

The interactions of sodium dodecyl sulphate with ovalbumin in aqueous solution at room temperature are described for a wide concentration range of both substances. A phase diagram covering a wide range of concentrations shows a total of five different morphologies. Dynamic light scattering of the samples from each morphology offered better understanding of the different structures (between three and four) present in the solution. The amount of ovalbumin present in the solution was confirmed with differential scanning spectroscopy, while the interactions between sodium dodecyl sulphate and ovalbumin were interpreted by zeta potential and electrical conductivity measurements.     

Microemulsion photopolymerization of methacrylates stabilized with sodium dodecyl sulfate and poly(N-acetylethylenimine) macromonomers

Methyl methacrylate and butyl methacrylate were polymerized in oil-in-water microemulsions that were stabilized by sodium dodecyl sulphate (SDS). A poly(N-acetylethylenimine) (PNAEI) macromer was also included in the recipe, as a cosurfactant and a comonomer. Polymerizations were initiated by UV-irradiation. The average diameters of latex particles, obtained by STM, were in the range of 17-200 nm. The experimental data evidenced that the particle size was mainly dependent on the SDS/PNAEI ratio. Polymerization yields were around 75-85%. The synthesized copolymers have viscosity average molecular weights in the range of 2.1-2.4×10⁶ and glass transition temperatures of 38.0-43.5°C, lower than those obtained without using PNAEI. The investigation by means of FTIR and 1H-NMR techniques revealed that PNAEI was incorporated into the nanoparticles.     

烷基硫酸钠对MMA种子乳液聚合的影响

研究了烷基硫酸钠纯度，烷基碳链分布对甲基丙烯酸甲酯种子乳液聚合反应的影响。结果表明，烷基硫酸钠中乙醇不溶物含量的增加，可提高ＭＭＡ乳液聚合反应速度，在采用Ｋ２Ｓ２Ｏ８－ＮａＨＳＯ３－Ｃｕ＾２＋三元氧化－还原引发体系的ＭＭＡ乳液聚合中，Ｆｅ＾２＋降低反应速率，而Ｆｅ＾３＋则提高聚合反应速率；     

Effect of sodium metasilicate on natural flotability of coal

The effect of the quantity of sodium metasilicate and conditioning time in one set of experiments, and the effect of the solution concentration of sodium metasilicate, added at the same dosage and conditioning time to coal slurry, on flotability of a typical Indian coal in another set of experiments are studied. Two sets of 3² full factorial experiments are carried out to assess the effects of the aforementioned variables. The generated data are analyzed quantitatively and explained qualitatively. At 0.1% (w/v) solution concentration of solution added (0.02 g/kg) and 8 min conditioning time, sodium metasilicate acted as activator for kaolinite, whereas at 1.0% (w/v) solution concentration (0.2 g/kg), it acted as dispersant. The best observed condition of depressant is obtained at an added concentration of 10.0% (w/v, 0.2 g/kg) and 8 min conditioning time. The desired effect of the sodium metasilicate can be achieved by controlling its quantity, solution concentration added, and conditioning time.     

Determination of DNA using sodium 9,10-anthraquinone-2-sulfonate as an in situ photochemical fluorescence probe

An in situ photochemical fluorescence probe method for the determination of DNA with sodium 9,10-anthraquinone-2-sulfonate (AQS) as a photochemical fluorescence probe was developed. It was based on the conversion of AQS into an intensively fluorescent product by irradiating with UV radiation. The photochemical reaction is retarded by DNA. The determination can be carried out by measuring the fluorescence intensity at a fixed time. The calibration graph was linear in the range 0–80 ng ml⁻¹ calf thymus (CT) DNA (r = 0.9991), the limit of detection was 3.2 ng ml⁻¹ CT DNA (n = 9). The kinetic behaviour of the photochemical reaction and the effects of experimental conditions were investigated and discussed in detail. The results of absorption spectra and competitive binding experiments suggested the interaction between AQS and DNA to be intercalative.     

Are the pyrazolines formed from the reaction of [60]fullerene with alkyl diazoacetates unstable?

[60]Fullerene-fused pyrazolines 1 were prepared by the reaction of C₆₀ with alky diazoacetates under the solid-state high-speed vibration milling conditions as well as in toluene solution. Pyrazolines 1 were stable in refluxing toluene and its thermolysis process in 1,2-dichlorobenzene was investigated, the decomposition rates and activation energies of pyrazolines 1 were obtained. The current work demonstrated that the liquid-phase reaction of C₆₀ with alkyl diazoacetates undergoes via 1,3-dipolar cycloaddition pathway at room temperature, or proceeds via carbene mechanism at a temperature of refluxing toluene, thus clarifies the previous ambiguity of its reaction mechanism.