Efficient microwave induced direct α-halogenation of carbonyl compounds

A novel and direct method for the synthesis of α-halocarbonyl compounds using sequential treatment of carbonyl compounds with [hydroxy(tosyloxy)iodo]benzene followed by magnesium halides under solvent-free microwave irradiation conditions is described.     

Synthesis and Structure of Novel Organocycloborates

A series of α,ω‐boryl(bromo)alkanes of the general formula R₂B? (CH₂)_n? Br (n=3, 4, 5, 6) was obtained in high yield following a standard hydroboration protocol. Upon treatment with Mg turnings and formation of the respective Grignard species, all alkanes with n=4 to 6 underwent an unprecedented boron‐centered cyclisation reaction with formation of boratacyclopentanes, ‐hexanes, and ‐heptanes, respectively. All new compounds were isolated in high yields as colourless, crystalline materials and characterised in solution by multinuclear NMR spectroscopy. Four representative examples were chosen for X‐ray diffraction studies, thus providing the first structurally characterised ring systems of that size at a tetraalkyl borate centre.     

Diagramme polythermique du systeme ternaire H2O—Al(NO3)3—Mg(NO3)2

The solid—liquid equilibria of the ternary system H₂O—Al(NO₃)₃—Mg(NO₃)₂ were studied at –30, –20, –10 and 0°C by using a synthetic method which allows to detemine all the characteristic points of isothermal sections. The stable solid phases which appear are respectively: ice, Al(NO₃)₃·9H₂O, Mg(NO₃)₂·9H₂O and Mg(NO₃)₂·6H₂O. Neither double salts nor mixed crystals are observed in the temperature and composition field studied. Polytherm diagram layout show two invariant transformations correspond with an eutectic point and a peritectic point.This revised version was published online in November 2005 with corrections to the Cover Date.     

Synthesis of poly(p‐phenylene sulfide) from bis(4‐bromophenyl) disulfide

Improved reaction conditions for the preparation of poly(p‐phenylene sulfide) (PPS) directly from bis(4‐bromophenyl) disulfide (BBD) have been established. Heating BBD with magnesium metal afforded only a low molecular weight polymer. PPS with a melting temperature around 280 °C was obtained from BBD in the presence of sodium carbonate or zinc metal. The best results were obtained with the addition of a catalytic amount of KI to the zinc–BBD mixture. Polymers prepared by the above methods are semicrystalline and dissolve in 1‐chloronaphthalene and have properties comparable to commercial PPS. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 900–904, 2006     

红外光谱法研究含CeSt3的LDPE膜紫外光氧降解

报道了硬脂酸铈（ＣｅＳｔ_３）、及其在各种浓度、或不同温度、或延长贮放时间下含ＣｅＳｔ_３的低密度聚乙烯（ＬＤＰＥ）膜紫外光氧化降解过程的红外光谱。结果表明，只要在ＬＤＰＥ膜中加入０．１ｗｔ＋％～０．３ｗｔ＋％ＣｅＳｔ_３光敏剂，即可控光降解ＬＤＰＥ膜的寿命。     

A microcalorimetric study of the association of hexacyanoferrate(II) ions with calcium and magnesium ions in aqueous solution

Using flow microcalorimetry, the ion association reaction M²⁺(aq)+Fe(CN) ₆ ^4– (aq)=MFe(CN) ₆ ^2– (aq) (M=Ca, Mg) has been studied at 25°C over the ionic strength range 0.02 to 0.08 mol-dm^–3. Analyses of the data to obtain H^o, the enthalpy change at infinite dilution, are described. The value obtained for H^o is sensitive to the kind of functions used to correct for non-ideal behavior.     

Quantitative thermogravimetric analysis of binary mixtures

Thermogravimetric analysis is used to determine the amounts of Mg(OH)₂ and Mg(CH₃COO)₂in a mixture thereof. The application and suitability of different analysis methods are discussed. In the first method the mass losses in the temperature ranges as indicated by the decomposition of the pure compounds were used. Results obtained using these temperature ranges were unusable. The percentage mass losses due to the decomposition of Mg(OH)₂ and Mg(CH₃COO)₂ were then determined in a second method using the minimum in the derivative mass vs. temperature curves. The results obtained by this method compared well with the actual values for mixtures containing more than 15% magnesium acetate. The third method employed the total experimental mass loss of both decomposition reactions. The results obtained using this method compared well to the actual values, giving a R ² value of more than 0.99. This method of using the total mass losses can however only be used for binary mixtures that consist only of magnesium hydroxide and magnesium acetate. This revised version was published online in August 2006 with corrections to the Cover Date.     

A study of the formation of silica-supported mixed magnesium-manganese spinel oxides from multicomponent gels

The effects of thermal treatment on composite materials prepared by the gelation of sols comprising large concentrations of metal oxide precursor salts have been investigated, in order to determine the compositional and thermal requirements for forming spinel magnesium manganates in such systems. The preparative technique has been found to give rise to derived gel materials in which the metal oxide phase, in the form of regular spherical particles, is dispersed throughout a continuous silica matrix. Silica-supported mixed magnesium and manganese spinel oxide phases were obtained for systems comprising at least 30 wt% metal nitrate after heating to temperatures between 700 and 850°C, but not without concomitant formation of Mn₂O₃ and modification of the silica network by magnesium.     

血镁水平与糖尿病肾病

为探讨糖尿病肾病 (DN)患者血镁水平 ,以 1 5 9例 2型糖尿病 (T2DM)患者为研究对象 ,用xylidylblue比色法测定了其正常白蛋白尿期、微量白蛋白尿期 (早期DN)、临床DN及晚期DN血镁水平 ,与 2 0例正常对照组相比较 ;同时将 1 1 0例DN患者分为肾功能不全代偿组、失代偿组和肾功能衰竭组 ,将其血镁水平与 1 0 2例慢性肾小球肾炎 (CGN)患者相比较 ,组间比较采用t检验 ;对 79例T2DM正常白蛋白尿期及微量白蛋白尿期患者尿白蛋白排泄率 (UAER)与血镁水平进行了等级相关分析。结果表明 ,T2DM正常白蛋白尿期、早期DN及临床DN血镁水平降低 ,晚期DN血镁水平升高 ,各组与正常对照组相比存在显著性差异 (P <0 0 5或P <0 0 1 ) ;T2DMDN及CGN肾功能不全代偿期、失代偿期及肾功能衰竭期血镁水平渐升高 ,且肾功能处于同一期的DN和CGN相比 ,前者血镁水平均较后者显著降低 (P <0 0 1或P <0 0 5 ) ;T2DM正常白蛋白尿期和微量白蛋白尿期血镁水平与UAER呈负相关 (r=0 5 47,P <0 0 1 )。提示T2DM患者肾功能正常时存在低镁倾向 ,但晚期DN血镁水平升高 ;随着肾功能不全进展 ,DN和CGN患者血镁水平升高 ,但前者血镁水平仍较后者低 ,镁代谢紊乱与DM及其并发症的相互关系有待进一步研究 ;血镁水平测定可否作为DN的早期诊断指标亦     

Supplementation with Magnesium Salts—A Strategy to Increase Nutraceutical Value of Pleurotus djamor Fruiting Bodies

The use of substrates supplemented with minerals is a promising strategy for increasing the nutraceutical value of Pleurotus spp. The current research was performed to analyze the effect of substrate supplementation with magnesium (Mg) salts on the Mg content, biomass, and chemical composition of pink oyster mushroom (Pleurotus djamor) fruiting bodies. Before inoculation, substrate was supplemented with MgCl₂ × 6 H₂O and MgSO₄, both salts were applied at three concentrations: 210, 420, and 4200 mg of Mg per 2 kg of substrate. The harvest period included three flushes. Substrate supplementation with 4200 mg of Mg caused the most significant decrease in mushroom productivity, of about 28% for both Mg salts. The dry matter content in fruiting bodies was significantly lower in the treatment in which 210 mg of Mg was applied as MgSO₄ in comparison to the control. Supplementation effectively increased the Mg content in fruiting bodies of P. djamor by 19–85% depending on the treatment, and significantly affected the level of remaining bioelements and anions. One hundred grams of pink oyster fruiting bodies, supplemented with Mg salts, provides more than 20% of the Mg dietary value recommended by the Food and Drug Administration (FDA); thus, supplementation can be an effective technique for producing mushrooms that are rich in dietary Mg. Although P. djamor grown in supplemented substrate showed lower productivity, this was evident only in the fresh weight because the differences in dry weight were negligible. Mg supplementation increased the antioxidant activity of the fruiting bodies, phenolic compounds, and some amino acids, including L-tryptophan, and vitamins (thiamine and l-ascorbic acid).