Ruthenium(Ⅲ) chloride as an efficient catalyst for the synthesis of perimidine derivatives under mild conditions

Various biologically important perimidine derivatives have been synthesized efficiently from various ketones and naphthalene- 1,8-diamine by using a catalytic amount of RuCl_3(1 mol%).This method is a very simple and high yielding reaction for the synthesis of perimidine derivatives.

Synthesis and structure characterization of diethyldiallylammonium chloride

The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of diethylallylamine (DEAA), and drying and temperature on the synthesis of DEDAAC were investigated. The content of in-process product DEAA was determined by non-aqueous titration. The structure of product DEDAAC was identified with IR, 1 H NMR and elemental analysis. The results show that adding allyl chloride and sodium hydroxide alternately can increase the yield of DEAA and decrease by-products. In further synthesizing of DEDAAC from DEAA, the step of drying DEAA is very necessary. When DEAA is dried by solid sodium hydroxide, good columnar crystals with a high purity(mp 199.5-201.0 ℃) are obtained; when DEAA is undried or the content of water in DEAA is above 20%, only platelets with bad quality are obtained even without crystals. The suitable synthesis conditions for DEAA and DEDAAC are 35 ℃, 6 h and 40 ℃, 36 h, respectively, and their yields are 69.7% and 67.3%, respectively.

Synthesis of Chlorosulfonyl-containing Pyrazolone Azo Compounds with Thionyl Chloride-DMF System

Chlorosulfonyl-containing pyrazolone azo compounds (2a, 2b) have been prepared by reaction of the corresponding sodium sulfonate (1a, 1b) with thionyl chloride in the presence of a catalytic quantity of N,Ndimethylformamide in dry benzene. The effects of reaction temperature, time, catalyst and solvent amount on the yield of 2a and 2b were investigated. The results show that chlorination of 1a and 1b under optimal conditions gives 2a and 2b in 95.5% and 99.2% yield respectively. The given method is facile and suitable for large-scale synthesis.

Strontium chloride-catalyzed one-pot synthesis of 4(3H)-quinazolinones under solvent-free conditions

Strontium chloride was used as an efficient and recyclable catalyst in one-pot condensation of anthranilic acid, ortho esters and amines leading to the formation of 4（3H）-quinazolinone derivatives in good yields at room temperature under solvent-free conditions.

Study on the Synthesis of Phenylacetic Acid by Carbonylation of Benzyl Chloride under Normal Pressure

The influences of some factors on the yield of phenylacetic acid in thecarbonylation of benzyl chloride were studied in this paper. These factors included the variety andcontent of catalyst, and that of solvent, way of material feeding, reaction temperature, sodiumhydrate concentration, triphenylphosphine content, presence of surfactant, the ratio of organicphase volume to aqueous phase volume etc. The optimum reaction conditions were found to be: with aone-time pour of 0.15 g Pd(PPh_3)_2Cl_2, 0.24 g PPh_3, 75 ml NaOH of 3.5 mol/L, 20 ml benzylchloride and 55 ml n-butyl alcohol, and the reaction was carried out at 50℃ for about 3 hours. Theas-obtained yield of phenylacetic acid was as high as 97.6%. In addition, the influences of thepresence of phenylacetic acid and air in the reaction system were also studied. The results showedthat the presence of air in the system and the entrainment of phenylacetic acid in the circulatingorganic phase had great influence on the reaction rate, the stability and performance of catalystand the yield of phenylacetic acid.

Influence of chloride salts on hydrogen generation via hydrolysis of MgH_2 prepared by hydriding combustion synthesis and mechanical milling

The effects of chloride salts(NaCl,MgCl2and NH4Cl)on the hydrolysis kinetics of MgH2prepared by hydridingcombustion synthesis and mechanical milling(HCS+MM)were discussed.X-ray diffraction(XRD)analyses show that high-purityMgH2was successfully prepared by HCS.Hydrolysis performance test results indicate that the chloride salt added during the millingprocess is favorable to the initial reaction rate and hydrogen generation yield within60min.A MgH2?10%NH4Cl composite exhibitsthe best performance with the hydrogen generation yield of1311mL/g and a conversion rate of85.69%in60min at roomtemperature.It is suggested that the chloride salts not only play as grinding aids in the milling process,but also create fresh surface ofreactive materials,favoring the hydrolysis reaction.

Synthesis and Crystal Structure of 4-tert-Butyl-6-(4-chlorophenyl)-3,6-dihydro-2H-1,3-thiazin-2-iminium Chloride

The title compound, 4-tert-butyl-6-（4-chlorophenyl）-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride （C14H18C12N2S）, has been synthesized by the reaction of 1-（4-chlorophenyl）- 4,4-dimethylpent-1-en-3-one with thiourea, and its crystal structure was determined by single- crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P211c with a = 16.3064（11）, b = 9.4471（6）, c = 11.2626 （8）A, β = 108.400（1）°, Z = 4, V = 1646.28（19） A^3, Mr = 317.26, Dc = 1.280 g/cm^3, S = 1.078,μ = 0.510 mm^-1, F（000） = 664, the final R = 0.0514 and wR = 0.1412 for 3210 observed reflections （I 〉 2σ（I））. The thiazine ring system displays a twisted boat conformation, and three N-H,..Cl hydrogen bonds exist in the crystal. The combination of two N-H...Cl hydrogen bonds generate an R2^1 （6） ring.

The Synthesis of Tertiary Amides by theReaction of Adducts of Schiff Bases andAcyl Chlorides with Allylsamarium Bromide

Adducts of Schiff bases and acyl chlorides react with allylsamarium bromide to afford the corresponding tertiary amides.

SYNTHESIS AND CHARACTERIZATION OF THE MIXED LIGAND COORDINATION COMPOUND FROM RARE EARTH CHLORIDE AND THE NEUTRAL LIGANDS CONTAINING NITROGEN

The method of synthesizing ternary solid mixed ligand complexes from 1,10-phenanthroline, 2,2’-bipyridyl is reported. The series of complexes have been characterized by elemental analysis, infrared spectra, DSC-TGA analyses and molar conductivity. The results agree with the general formula LnL1L2Cl3·nH2O （Ln=La,Pr,Nd,Sm, Eu; Gd, Dy, Er, Tm, L1=phen, L2=bipy, n= 1,2,3）.

REACTION OF FERROCENOYL CHLORIDE WITH [Et_(?)NH] [μ-CO)(μ-RS)Fe_2(CO)_6]COMPLEXES SYNTHESIS AND STRUCTURE OF Fe_2(CO)_6COMPLEXES WITH BRIDGING FERROCENOYL LIGAND

Reaction of ferrocenoyl chloride with [Et;NH] [（μ-CO）(μ-RS) Fe;=（CO）;] complexes gave bridging ferrocenoyl complexes（μ-FcCO）(μ-RS)Fe;（CO）;（Fc=ferrocenyl, R=Et, i-Pr, n-Bu, t-Bu, Ph）.The structures of all new complexes were characterised by;HNMR, IR and MS.

A NEW SYNTHESIS OF SULFONES VIA THE ZINC—ASSISTED COUPLING OF ARENESULFONYL CHLORIDE WITH ALKYL HALIDES

Arenesulfonyl chloride undergoes a facile one-pot coupling reaction with active halides assisted by zinc to give the corresponding sulfones in acceptable yields.

SOLID-LIQUID PHASE TRANSFER AND COBALT OR PALLADIUM COMPLEX CATALYZED SYNTHESIS OF ANHYDRIDES FROM ACYL CHLORIDES

Acyl chloride can efficiently be converted into anhydride under solid liquid phase transfer catalysis by using bis(triphenylphosphine)cobalt dichloride or bis(triphenylphospine)palladium dichloride as the catalyst.

Synthesis and Characterization of Poly [2,2-( m-phenylene) -5,5-bibenzimidazole] in 1-butyl-3-methylimidazolium Chloride

Poly[ 2, 2-（m.phenylene） -5, 5-bibenzimidazole] （mPBI） were synthesized by mixing 3, 3＇, 4, 4＇-tetraaminobiphenyl and isophthallc acid in 1 -butyl-3 -methyUmidazolinm chloride （ E BMIM] CI）. Intrinsic viscosity of mPBI polymers was 0.67 dL/g which was measured in 96% sulfuric acid. The polymer was characterized by Fourier transform infrared spectroscopy （FTIR）, nuclear magnetic resonance （ 1H-NMR ）, and thermogravimetric analysis （TGA）. The effects of polymerization conditions on the intrinsic viscosity of mPBI were investigated. It showed that the molecular weight of polymer mainly depended on pre-reaction time and reaction temperature. Comparison of structure and properties of mPBI synthesized in ionic liquids（ILs） and polyphosphoric acid was also reported. It indicates that the ionic liquids are a kind of good solvents in synthesis process of m_PBI and ionic liquids mainly affect molecular weight of mPBL

Synthesis of lanthanum tris (mono-i-octyl phthalate) and its thermal stability for polyvinyl chloride

A novel type of thermal stabilizer-lanthanum tris (mono- i -octyl phthalate) (LTMP) was synthesized by double-decomposition reaction o f sodium mono- i -octyl phthalate with lanthanum chloride at 60 ℃. Sodium m ono- i -octyl phthalate was prepared by sodium hydrate and mono- i -octy l phthalate prepared by reaction of isooctyl alcohol and phthalic anhydride in th e presence of sulfuric acid catalyst at 110 ℃. The yield of lanthanum tris (mon o- i -octyl phthalate) is about 84.5%. Its thermal stabilities were measured by heat-ageing oven test when incorporated into PVC. The experimental results show that the heat stability time is about 40min at 190 ℃ when adding 3phr (pe r hundred resin) to PVC. The thermal stability of this product is better than th at of Ca-Zn complex and basic lead salt stabilizers, and equal to that of dibut yltin dilaurate.

Mechanism of scaling on oxidation reactor wall in TiO_2 synthesis by chloride process

The mechanism of scaling on the oxidation reactor wall in TiO2 synthesis process was investigated. The formation of wall scale is mostly due to being deposited and sintered of TiO2 particle formed in the gas phase reaction of TiCl4 with O2. The gas-phase oxidation of TiCl4 was in a high temperature tubular flow reactor with quartz and ceramic rods put in center respectively. Scale layers are formed on reactor wall and two rods. Morphology and phase composition of them were characterized by transmission electron microscope(TEM), scan electron micrographs(SEM) and X-ray diffraction(XRD). The state of reactor wall has a little effect on scaling formation. With uneven temperature distribution along axial of reactor, the higher the reaction temperature is,the thicker the scale layer and the more compact the scale structure is.

SYNTHESIS，PROPERTY AND HEAT STABILITY FO RPOLYVINYLCHLORIDSOFANTIMONYTRIS（MERCAPTOACIDESTER）

Antimony mercaplde heat stabilizer for polyvinyl chlorideis synthesized from antimony trioxide and mercaptocarboxylic acid esters, HS(CH2).COoi-C8H17 (n=1～2) at 100～115 C In the presence of 0. 5%～1 % an organic acid catalyst. Some physicochemicalconstants of the compounds, such as density and refractive index, aredetermined. The complexes are hydrolabll in aqueous solutions andthe bond of Sb-S is weaker than that of Sb-o. The forming bondproperty of antimony tris (mercaptoacid ester ) has been elucidatedby measurement of infrared spectra in comparison with mercaptocarboxylic acid esters. The polyvinyl chloride resins containing antimony mercaptide heat stabilizers, do not darken at elevated temperatures and exhibit a high degree of stability. It is proposed that mercaptocarboxylic acid ester freeradicals can esterify PVC microradicals at carbon atoms with upaired electrons.

Synthesis of arbutin by two-step reaction from glucose

Arbutin was synthesized from glucose by two-step reaction below: (a) 2,3,4,6-tetra-O-acetyl-α-D-glucosyl chloride or bromide was prepared by glucose and acetyl halide (chloride or bromide), (b) 2,3,4,6-tetra-O-ace-tyl-α-D-glucosyl halide (Cl, Br) reacted with hydroquinone, methanol as solvent at pH=9.5-10.0.

Synthesis of allylamine in ethanol

Allylamine was prepared from the ammonolysis of allyl chloride or the reaction of allyl chloride with hexamethylenetetramine in ethano l. The selectivity of allylamine was improved from 21.4% to 67.6% when the re action was carried out in ethanol instead of liquid ammonia. At the same time, the selectivity of allylamine was increased from 13.3% to 67.6% when the molar ratio of NH3 to allyl chloride was increased from 4.5∶1 to 25∶1.However, t he reaction of allyl chloride and hexamethylenetetramine in ethanol produced all ylamine with high selectivity （100%） and high yield （87%）.The synthesis of allyl amine from the reaction of allyl chloride and hexamethylenetetramine in ethanol was more straightforward and convenient.

Synthesis of 4'-Methoxy Flavone

Synthesis of 4'-methoxyflavone, first by the reaction of 4 - methoxy acetophenone enamine with heptanedioyl chloride, then by dehydrogenation, is described.