• Volume 34,Issue 3,2017 Table of Contents
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    • >Review and monographs
    • The research progress of dispersion based on aqueous ink

      2017, 34(3).

      Abstract (1471) HTML (0) PDF 0.00 Byte (2) Comment (0) Favorites

      Abstract:Combining with the domestic and foreign research present, the article summarized and analyzed the aqueous ink's dispersion stability mechanism and the main factors influencing the dispersion. The results shows that wettability of pigment, pigment particle size and particle size distribution, the properties of resin, the viscosity and pH value of the ink are closely related to the dispersion of aqueous ink; Then, this paper expounded several main ways to improve dispersion and dispersion stability, including the surface modification of pigment, using surfactant or super dispersant, morphology design of pigment and the pre dispersion of pigment. Furthermore put forward that with the further adjustment of the national industry, environment-friendly aqueous ink will gradually replace the traditional solvent based ink, so improving the quality of water-based ink has been the first priority.

    • >Functional materials
    • Preparation and Characterization of PDEGMA-b-POVNGA@AuNPs

      2017, 34(3).

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      Abstract:The PDEGMA-b-POVNGA@AuNPs complex was prepared by a combination of enzymatic synthesis , reversible addition-fragment chain transfer (RAFT) polymerization protols and the “one-pot”method. The targeted glycomonomer 6-O-vinyladipoyl-α-D-galactose (OVNGA) and thermoresponsive diethyleneglycol methacrylate (DEGMA) as the monomers to form PDEGMA-b- POVNGA, the thermoresponsive glycopolymer. Then the PDEGMA-b-POVNGA combined with gold nanoparticals(AuNPs) to prepared PDEGMA-b-POVNGA@AuNPs complex by S—Au bond. The structure of PDEGMA-b-POVNGA was characterized by 1HNMR, FTIR and GPC. UV-visible spectroscopy tests showed that the low critical solution temperature (LSCT) of PDEGMA-b-POVNGA is about 35 ℃. Dynamic light scattering (DLS) demonstrated that the average diameter of AuNPs is 25nm. The PDEGMA-b-POVNGA@AuNPs complex was characterized by TEM. The result proved that the block polymer has grafted in the surface of AuNPs. UV-visible spectroscopy tests showed that the LSCT of PDEGMA-b-POVNGA@AuNPs is about 34.5 ℃. PDEGMA-b-POVNGA@AuNPs may have potential as functional drug carriers.

    • Preparation and Properties of Slow-released System of Acetamiprid/Schiff Base Modified Attapulgite

      2017, 34(3):0-0.

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      Abstract:Schiff base copper ion complex modified attapulgite (Cu2 -Sal-ATP) was prepared by post-grafting method. Acetamiprid loading into the pores of attapulgite(ATP) was performed by the immersion method. The modified Attapulgite were characterized by fourier transform infrared spectroscopy(FTIR), N2 adsorption-desorption, scanning electron microscopy(SEM), X-ray diffraction (XRD) and differential scanning calorimeter(DSC). The drug loading content and drug release kinetic were also systematically studied. The results showed that the loaded acetamiprid was apparently in amorphous form, and that the loading process did not change the structure of the carrier. The loading content of acetamiprid was increased with the organic modification of ATP, Cu2 -Sal-ATP has the highest loading content among the unmodified and organically modified ATP. The adsorption process for acetamiprid follows the pseudo-second-order kinetic model. The Cu2 -Sal-ATP/acetamiprid system exhibits better slow-release properties than schiff base modified ATP(Sal-ATP)/acetamiprid system, and their releasing curves could be described by Korsmeyer-Peppas equation.

    • >Surfactants
    • Synthesis and Application of a New Type of Organic Silicone Defoamer

      2017, 34(3).

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      Abstract:The organosilicon high polymers(modified silicone oil) were synthesized by using allyl alcohol polyoxyethylene polyoxypropylene ether (FB), long-chain alkyl esters and hydrogen silicone hydrosilation(PHMS) addition change. And using by infrared spectrum and nuclear magnetic resonancespectrum of its structures have been characterized . A silicone defoamer was prepared with the organosilicon high polymer as active ingredient. It is discussed on the stability , surface tension, defoaming performance of the long -chain alkyl ester segment of its length . The results show that the defoamer performs the most stability, the most uniform particle size distribution and optimal application performance when synthetized with methacrylate tetradecyl methacrylate and allyl alcohol polyether modified silicone oil. The particle size of the defoamer mainly spread in 260 nm. The defoaming time of the defoamer is 6 s, 4 s, 12 s respectively when it is in 5% mass fraction dodecyl sodium solution, 5% detergent solution and black liquor (30% lignin). The defoamer shows better property than RX-504 and 850E coming from .China and Germany.

    • Synthesis, Characterization and Properties of Palmitamidopropyl Betaine Amphoteric Surfactant

      2017, 34(3).

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      Abstract:The palmitamidopropyl betaine (PAPB) type amphoteric surfactant was synthesized by sodium choloroacetate and palmitamidopropyldimethyl tertiary amine that was synthesized by an amidation with palmitic acid and N,N-dimethyl-1,3-propanediamine as raw material. The effects of reaction temperature and time, the molar ratio of palmitic acid to N,N-dimethyl-1,3-propanediamine, the amount of catalyst, 4 A molecular sieves on conversion of palmitic acid were studied. Meanwhile, the structure of product was characterization by FTIR and 1HNMR, and properties of palmitamidopropyl betaine and the mixed surfactant systems were investigated. The results showed that the optimum conditions of amidation reaction were screened out as follows: reaction temperature of 160℃ and reaction time of 10 h, the molar ratio of N,N-dimethyl-1,3-propanediamine to palmitic acid 1.05:1, the amount of catalyst KOH of 0.5%. Under the above conditions, the conversion of palmitic acid was 92.41%. The critical micelle concentration and surface tension of palmitamidopropyl betaine were 1.12×10-4 mol•L-1 and 31.63 mN•m-1, respectively, and its solubilization capacity of benzene was 4980mL/mol.

    • A Star-shaped Anionic Surfactant:Synthesis, Emulsification Properties and Interfacial Tension at the Crude Oil-Water Interface

      2017, 34(3):0-0.

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      Abstract:In the research, a star-shaped surfactant was synthesized through the chlorination reaction, alkylation reaction and sulfonation reaction of triethanolamine. The star-shaped surfactant synthesized is composed of three hydrophobic chains and three sulfonate hydrophilic groups. Study found that the surfactant has high surface activity with CMC of 4.93×10-5 mol/L and interfacial tension of 32.0 mN/m. At the same time, the effects of the star-shaped surfactant’s concentration and alkalinity (NaOH concentration) on the interfacial tension of the crude oil-water interface would be discussed. It’s indicated in the research that a small amount of star-shaped surfactant can effectively reduce the interfacial tension of crude oil-water interface. When the surfactant concentration was 0.1 g/L and NaOH concentration was 0.5 g/L, interfacial tension of crude oil-water system at 50 ℃ dropped to 1.1×10-4 mN/m, which suggested that the surfactant reached the ultra-low interfacial tension, which can satisfy the requirement of surfactants for oil displacement. And the self-emulsification experiment indicated that the surfactant had excellent emulsification performance. When the surfactant concentration was 0.1 g/L, the crude oil would be turned into O/W emulsion with particle size of 5 ~ 20 μm.

    • >Electronic chemicals
    • Effect of ZnF2 Coating on LiNi0.5Mn1.5O4 Cathode Material for Lithium-ion Batteries

      2017, 34(3).

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      Abstract::LiNi0.5Mn1.5O4 of a 5 V cathode material was prepared by a sol-gel method, and subsequently coated with ZnF2 as a buffering layer. XRD test showed that ZnF2 coating treatment have no effect on the crystal structure of LiNi0.5Mn1.5O4. EDS,SEM,TEM test indicated that 2wt% ZnF2 formed uniform layer on the surface of LiNi0.5Mn1.5O4 with a thickness of 7 nm.The electrochemical performance of the pristine LiNi0.5Mn1.5O4 and LiNi0.5Mn1.5O4 with various coating levels of 1wt%, 2wt%, 3wt% ZnF2 were tested and compared in half-cells. The ZnF2 coating layer decreased the interaction between the electrolyte and the cathode material, greatly stabilized the electrode surface,thus improving the electrochemical performances. LiNi0.5Mn1.5O4 with an optimized coating level of 2wt% ZnF2 exhibited the best performances, delivering a discharge capacity of 109 mAh·g-1 and maintaining 79.7% capacity retention at 0.2 C after 200 cycles. After cycled 500 cycles at a high current of 5 C, it still showed a high 85.6% capacity retention of 85.6% with a discharge capacity of 94.2 mAh·g-1.

    • >Modernization technology of traditional Chinese medicines
    • Optimization of ultrasonic/microwave assisted extraction of Sophora tonkinensis Gapnep. flavonoids by genetic algorithm and their antioxidant activies and antibacterial activities

      2017, 34(3).

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      Abstract:Objective To optimize the ultrasonic/microwave assisted extraction method of Sophora tonkinensis Gapnep. flavonoids by genetic algorithm, and to study their antioxidant activies and antibacterial activities. Methods Used the flavonoid yield as index, the solid-liquid ratio, ethanol concentration, microwave power and extraction time were tested by single factor test and orthogonal test design, and the technological conditions was optimized by genetic algorithm. The scavenging rates of S. tonkinensis Flavonoids on 1,1-diphenyl-2-picrylhydrazyl radical(?DPPH), superoxide anion radical (O2-?)and hydroxyl radical (?OH) were tested to evaluate the in vitro antioxidant activities. The peroxide value(POV) of S. tonkinensis flavonoids on lard, peanut oil and corn oil were tested to evaluate the in vitro anti-lipid activities. And the antibacterial activities of S. tonkinensis Flavonoids on 7 species of common bacteria were evaluated by filter paper disc diffusion method. Results The optimum technological conditions were as followed:the solid-liquid ratio was 24.9:1(mL/g),ethanol concentration was 87%, microwave power was 699 W, and extraction time was 3min. Under this conditions,the flavonoid yield was 10.38mg/g, which was 99.69% of the model predictive value. The antioxidant activity study showed that the S. tonkinensis flavonoids possessed good antioxidant activities, the DPPH?, O2-?and?OH scavenging rates were 96.38% 91.35% and 82.23% when the flavonoid concentration was 30礸/mL, respectively. The in vitro anti-lipid study showed that S. tonkinensis flavonoids could obviously slow down the oxidation rates of lard, peanut oil and corn oil in the test time range, the anti lipid oxidation were equivalent to BHT with the same mass fraction. The antibacterial activity study showed that the S. tonkinensis flavonoids had good antibacterial activities on 6 species of common bacteria, and the order of antibacterial activities was Staphylococcus aureus, salmonella, shigella, Bacillus subtilis, Escherichia coli and yeast, but the study also showed that the S. tonkinensis flavonoids had no antibacterial activity on Aspergillus niger in the test range. Conclusion To optimize the extracting technical conditions by genetic algorithm was more reliable and more closer to practical production. The S. tonkinensis flavonoids possessed good antioxidant and antibacterial activities, which could be use as natural antioxidants and preservatives for food.

    • >Catalysis,separation and purification technology
    • Keggin-type Tin Mono-substituted Heteropolyacid Salt Catalyst in the Synthesis of Cyclohexanone

      2017, 34(3).

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      Abstract:Using sodium tungstate﹑cobalt acetate and stannic chloride as raw materials, Sn-substituted heteropoly acid potassium salt K7MⅡW11SnⅣO39OH (M =Co,Fe,Ni,Zn,Mn) and quaternary ammonium salt were synthesized by the acidification method, and characterized by Fourier transform infrared (FTIR), X-ray diffraction (XRD) and Inductively Coupled Plasma-Atomic Emission Spectrometry(ICP-AES). Its catalytic activity was measured in the oxidation of cyclohexanol to cyclohexanone with mass fraction 30% aqueous hydrogen peroxide as an oxidant. The conversion of cyclohexanol and the selectivity of cyclohexanone were found to be as high as 95.68% and 96.75% under the optimum conditions which the quantity of catalyst (C4H9)4NHxCoⅡW11SnⅣ was 0.25mmol, cyclohexanol was 0.05 mol, hydrogen peroxide was 0.2 mol, acetonitrile was 0.2 mol at 85℃for 2 h, and a possible reaction mechanism of the oxidation of cyclohexanol was concluded that transition metal Sn was act as catalytic active center.

    • Catalytic Performance of magnetic (CaO-MgO)@Fe3O4/C solid base catalyst for Glycerol carbonate production from Glycerol

      2017, 34(3).

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      Abstract:Magnetic heterogeneous catalyst ((CaO-MgO)@Fe3O4/C) was prepared for co-precipitation methods and magnetic core Fe3O4/C was reduced by activated carbon under N2 atmosphere. The reaction of glycerol carboante prepared using glycerol as a probe reaction, it is investigated that the catalytic performance of (CaO-MgO)@Fe3O4/C catalyst. With (CaO-MgO)@Fe3O4/C catalyst, glycerol carbonate yield reached 98.80% and glycerol conversion reached 95.20%. The (CaO-MgO)@Fe3O4/C catalyst was characterized by magnetic hysteresis loop, X-ray diffraction (XRD), CO2-TPD and transmission electron microscopy (TEM) and BET. The results indicated that Fe3O4/C was well wrapped (CaO-MgO); the (CaO-MgO)@Fe3O4/C catalyst exhibited good magnetic properties with high saturation magnetization (23.8emu/g) and the (CaO-MgO)@Fe3O4/C catalyst had strong basicity. The different reaction conditions on the yield of glycerol carbonate were investigated. The optimal reaction conditions were as follows: the reaction temperature was 85 oC and the reaction time was 1h, the molar ratio of DMC/glycerol was 5:1 and the catalyst dosage was 5.0wt. %. The catalyst still had steadily catalytic performance after 5 cycles with a high glycerol carbonate yield of 94.45%.

    • >Leather chemicals
    • Preparation of Schiff Base of Glyoxylic Acid and 2-Amino-1,4-Benzenedisulfonic Acid and its Application in Pickling

      2017, 34(3).

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      Abstract:A Schiff base rich in sulfonic acid group and carboxyl group was prepared by glyoxalic acid and 2-Amino-1,4-benzenedisulfonic acid and was treated as pickling auxiliary used in pickling process,swelling rate of acidic pelts, shrinking temperature of wet-blue leather, the content of Cr2O3 and of spent tanned liquor has been determined. Result shows: 2% pickling auxiliary(based on limed pelts weight, same below) was used in salt-free pickling, swelling degree of pelts pickled was about 4%, on this basis, 1% sodium chloride was added into pickling liquor, swelling phenomenon of pelts pickled was avoided. 4.5% chrome powder was applied to less-salt pickling chrome tanning, Ts of wet-blue leather could achieve to 105.5℃. Compared with traditional pickling chrome tanning process, the content of Cr2O3 and Cl- of spent tanned liquor significant were reduced from 3.305g/L和374.2mmol/L to 1.546g/L and 59.6mmol/L. Observation from ESEM showed that fiber uniformly dispersed, surface smooth, pores clear, and EDS showed chromium elements was uniformly distributed in cross section of pelts. Compared with traditional process, tensile strength, elongation at break and tear strength were up to 32.8MPa, 56.8% and 80.2N/mm respectively.

    • >Starch chemicals
    • Corrosion Inhibition of Cationic Cassava Starch Graft Copolymer for Steel in HCl solution

      2017, 34(3).

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      Abstract:Cationic cassava starch graft copolymer (CCSGC) was prepared by reacting cassava starch (CS) with acryl amide (AA) and dimethyl diallyl ammonium chloride (DMDAAC). The corrosion inhibition of CCSGC on the corrosion of cold rolled steel in HCl was studied by weight loss, open circuit potential (OCP)-time curves, potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and scanning electron microscope (SEM) methods. The results show that CCSGC exhibits outstanding inhibition effect for cold rolled steel in 1.0 mol/L HCl, and the inhibition efficiency values are higher than 92% at 20 ~ 50 oC even when the additive CCSGC concentration is as low as 50 mg/L. The inhibitive performance of CCSGC is better than the reactants of AA, CS, DMDAAC or AA/CS/DMDAAC mixture. The adsorption of CCSGC on steel surface obeys Langmuir adsorption isotherm, and it is an exothermic process that involves mixed adsorption accompanied by an increase of chaotic degree. CSGC is a mixed-type inhibitor that retards both anodic and cathodic reactions simultaneously, and the electrochemical mechanism is caused by "geometric blocking effect". EIS exhibits the depressed capacitive loop, and the charge transfer resistance increases with the concentration of inhibitor, while double layer capacitance decreases. SEM reveals that the corrosion of steel is prominently retarded after adding CCSGC to the media.

    • >Water treatment technology and environmental protection
    • Flocculation Effect of Amphoteric Keratin on the Leather Dyeing Fatliquoring Wastewater and Reusing the Flocs

      2017, 34(3).

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      Abstract:Amphoteric Keratin was made by 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and sodium chloroacetate.And study the Flocculation Effect on the Leather Dyeing Fatliquoring Wastewater in this paper.Laboratory work has been carried out to investigate the influences of amphoteric keratin dosage, pH value and flocculation time on the removal rate of CODcr and total Cr efficiency. Results showed that:when the flocculent dosage was 0.5g稬-1,pH 4.0 and flocculation time was 4h, removal of CODcr and total Cr from 18840mg稬-1,19.0225mg稬-1 to 3600mg稬-1 and 1.277mg稬-1,as well as the decolorization effect is obvious. The flocs were used to fill the chrome tanned leather after proper treatment.The results showed that the thickening rate was 7.32%,the tensile strengthen was strenghten as well as the elongation at break had good effect. what’s more ,it plays a good dispersion on the lether fibers and the reusing flocs are practial and effective.

    • The Study on Corrosion Inhibition Performance of Thiourea Base Rosin Imidazoline Quaternary Ammonium Salt for A3 Mild Steel

      2017, 34(3).

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      Abstract:Thiourea base rosin imidazoline quaternary ammonium salt was synthesized,and the structure of thiourea base rosin imidazoline quaternary ammonium salt was characterized by FT-IR and 13C NMR.The static weight-loss method,potentiodynamic polarization test,electrochemical impedance spectroscopy test and contact angle test were conducted to investigate the corrosion performance of target product for A3 carbon steel in the mass fraction of 15% hydrochloric acid solution.The adsorption film of the product was characterized by atomic force microscope test and X-ray electron spectroscopy test.The results showed that the corrosion inhibition efficiency of the product increases first and then decreases with the increase of the mass fraction of the product,and the highest inhibition efficiency reached 90.78% at the product mass fraction is the quality of hydrochloric acid 0.4%;This product acted as the mixed type corrosion inhibitor dominated by cathode;AFM and XPS results show that the target product can form inhibitor adsorption film on the surface of carbon steel.

    • >Rubber and plastics auxiliaries
    • Synthetic Process of Hindered phenolic Antioxidant 1330 via Strong-acidic Cation Exchange Resin

      2017, 34(3):0-0.

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      Abstract:Strong-acid cation exchange resins were employed to catalyze to synthesize 1,3,5-trimethyl-2,4,6-tris(3,5-di-tertbutyl-4-hydroxybenzyl)benzene(antioxidant-1330). During the reaction, a methanol-containing binary azeotrope mixture which was generated as by-product need to be distillated. The effect of type and quantity of resins, reaction time, repeated times of catalyst on the yield were investigated. Results of experiments show that the activity of big bore resins without water was higher than aquiferous ones. The most preferred conditions are as follow: n(3,5-di-tertbutyl-4-hydroxybenzyl methyl ether):n(mesitylene)=3.6:1, m(resin):m(3,5-di-tertbutyl-4-hydroxybenzyl methyl ether)=1.03:1, reaction temperature 40℃ and reaction time 2 h. The yield of UV-1330 is 85.7% which can be kept above 82% after repeat used 6 times. In this new process, there is no waste acid and the effluent can be reduced 50 to 60 percent compared with prior process.

    • >Oil field chemicals and petroleum additives
    • Study on preparation and application of composite viscosity reducer SDG-3 aimed at ultra-heavy oil

      2017, 34(3).

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      Abstract:In view of the problem of mining ultra-heavy oil is very difficult in Tahe oilfield, and traditional chemical methods for reducing viscosity of heavy petroleum fluids include oil-soluble and water-soluble viscosity reducers have their own limitations. In this work, a new effective composite viscosity reducer SDG-3 was developed, its performance of ability of dispersing heavy components, interfacial activity, emulsifying properties, viscosity reducing, salt and heat resistance, demulsification, et al, were evaluated. Experimental test show that, without the presence of water, the viscosity reducer SDG-3 with amounts of 1wt.% can provide a degree of viscosity reduction (DVR%) of 50% for the ultra-heavy oils tested, possessing the ability of dispersing heavy components in crude oil. A much lower oil-water interfacial tension (IFT) of 0.32 mN/m can be achieved when SDG-3 is added into water with a high salinity of 2.2×105 mg\L and heavy oil with viscosity of 1.81×105 mPa•s than the IFT of 27 mN/m without SDG-3. Emulsification capability of SDG-3 for ultra-heavy oil looks better than water-soluble viscosity reducer, the average droplet size of the oil in water (O/W) emulsion was 2.5μm. We can achieve more a degree of viscosity reduction (DVR) of 99% for Venezuela, CNOOC and Tahe (China) heavy oils when the emulsification occurs, which was better than traditional oil-soluble viscosity reducer whose DVR is 72.6%. SDG-3 has capacity of temperature-resistant 140 ◦C and salt-tolerant 2.2×105mg/L, respectively, having no influence on post-processing. Field tests of the new composite viscosity reducer are carried out in the Tahe oilfiled of Xinjiang province in China. The field tests show that 66.6 % less light oil is needed to dilute the heavy oil to the desired viscosity when the new viscosity reducer is used. On average, a 14.4% increase in the heavy-oil production rate can be obtained.

    • >Acrylic series chemicals
    • Preparation and Properties of Waterborne Polyurethane?acrylate Modified by 4-Maleimidophenol

      2017, 34(3):0-0.

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      Abstract:A series of 4-maleimidophenol modified anionic waterborne polyurethane—acrylate (MWPUA) emulsions were prepared by in-situ polymerization with isophorone diamine (IPDI), poly-caprolactone diol (PCL), 2,2-dimethylolpropionic acid (DMPA), trimethylol propane (TMP), 4-maleimidophenol (4-HPM), methyl methacrylate (MMA) and butyl acrylate (BA) as main raw materials. Structure and properties of polymer were characterized by FT-IR, TEM, XRD, TGA and tensile testing. The effects of the content of 4-HPM on the properties of MWPUA emulsion and its films were also studied. The results showed that latex particle is ball-like, and has a core-shell structure. When w(4-HPM)=3.0wt%, the average particle size was 97.8 nm with narrow particle size distribution. Compared with the pure waterborne polyurethane (WPU), the crystallinity and thermal stability of MWPUA latex film has improved. The maximum decomposition rate of film decreased 8.1%, the tensile strength was up to 24.9MPa, water contact angle reached 103.2? water absorption ratio was as low as 8.8%.

    • >Fine chemical intermediates
    • Microwave-assisted One-pot Conversion of 1-(2-Hydroxyphenyl)ethanone Oximes to Benzo[d]isoxazoles Catalyzed by Sodium 2-Chloro-2,2-difluoroacetate

      2017, 34(3).

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      Abstract:One-pot conversion of 1-(2-hydroxyphenyl)ethanone oximes to benzo[d]isoxazoles was achieved under microwave-assisted condition and catalyzed with sodium 2-chloro-2,2-difluoroacetate (SCDA). The effects of solvent, the amount of iodine, microwave power and reaction temperature on the reaction were considered. The optimized reaction conditions are: n(oximes):n(SCDA): n(K2CO3) = 1:1.5:1.5, in N,N-dimethylacetamide (1 mol/L for oximes), microwave power 300 W, reaction temperature 85 ℃, reaction time 35 min. Eight benzo[d]isoxazoles with different substituent groups were synthesized in 64%~93% yields under the optimized reaction conditions. The structures of all products were confirmed by the corresponding nuclear magnetic resonance spectrum (1HNMR) and mass spectrum (MS).