HONG Yu , SHEN Yi-ding , YANG Xiao-wu , LIU Guan-jun , ZHANG Lin
2013, 30(4).
Abstract:An ammonium gemini surfactant (C16-2-C16?Br-) was synthesized by Bromohexadecane and N,N,N′,N′-tetramethyl-ethylenediamine. The synthetic technology was optimized by single factor analysis method. The optimical synthesis condition was received when the molar ratio of Bromohexadecane and N,N,N',N'–tetramethyl- ethylenediamine was 2.1, reaction temperature and time were 80℃and 24h, respectively. The chemical structure was characterized by Infrared Spectroscopy and 1HNMR. The influencing factors, such as surfactant mass concentration, temperature and shear rate, on the viscosity behavior of C16-2-C16?Br- solution were investigated. The viscosity of the gemini surfactant solution increase with the rise of mass concentration, decline sharply and then essentially unchange with the increase of temperature and shear rate. The flow index was lower than 0.6, calculated by Ostwald-de Wale power-law equation, and it indicates that the solution is pseudoplastic fluid.
ZHU Li-fang , MA Li , LIU Xiong-min
2013, 30(4).
Abstract:The metabolic pathway for the degradation of cinnamic acid with Mucor sp. was studied by analyzing metabolites using GC-MS. β-phenethyl alcohol, for the first time, was detected as an intermediate in transforming cinnamic acid to acetophenone by Mucor sp. The metabolic pathway of cinnamic acid was supposed: epoxidation reaction was occurred on the double bond of cinnamic acid side chain to generate ethyl 2,3-epoxy-3-phenylpropionic acid, the epoxide was converted to β-phenethyl alcohol via decarboxylation and ring-opening reaction, lastly, acetophenone was produced from β-phenethyl alcohol via hydroxyl migration and oxidation reaction.
2013, 30(4).
Abstract:Lepidium meyenii Walpers (MACA), as famous supplement plant source in Cordilleras of South America , have been successfully carried out to be large-scale cultivated in Lijiang of Yunnan province of CHINA.This paper reported.that the differences of the main compounds of essential oils by steam distillation extraction , Petroleum ether leaching , and Ether extraction from Lepidium meyenii Walpers cultivated in Lijiang of Yunnan Province, and Ninety chemical components were analyzed and identified by gas chromatography/mass spectrometry (GC/MS). The Study results showed that the main compounds of essential oils by Petroleum ether leaching is 1,1-dimethylethoxy)methyl]- Benzene (26.00%),N-(phenylmethyl)- Acetamide(23.47%),Phthalic acid, hexyl octyl ester(23.49%); and that of steam distillation extraction is 1-isocyano-2-methyl- Benzene(81.80%), that of Ether extraction from steam essential oil of Lepidium meyenii Walpers cultivated in Lijiang is Benzyl nitrile (56.29%) .
2013, 30(4).
Abstract:Flavonoids were extracted from “Miliang Kiwifruit” root under ultrasonic assistance, using ethanol as extraction solvent. The technical conditions were investigated based on single factor and orthogonal tests. The hydroxyl radical-scavenging capacities and the antioxidative activities to oils and fats of the flavonoids extracts were assessed and compared with citric acid and Vc. The results showed that the optimal extracting conditions were obtained as follows:60% ethanol, 1:30 (g: mL) material-to-liquid ratio, 40 min of ultrasonic extracting time and 60 ℃ water-bath of ultrasonic temperature. Under the optimal conditions, extraction rate of total flavonoids was 1.5%. The scavenging capability on ?OH free radical increased with extracts concentration increasing. Furthermore, the antioxidant activity of flavonoids extracts was excellent for oils and fats.
XIONG Li-zhi , OU Yang-wen , LI Chun , ZHANG Xiao-rong
2013, 30(4).
Abstract:Abstract: The purification of flavonoids from Artemisia Annua L.was studied by macroporous adsorption resins and antioxidant activity of the flavonoidswas was investigated. The adsorption and desorption effects of AB-8, DM-101, DA-201, D-101, SD-401 on flavonoids from Artemisia Annua L. were compared. Results show that the D-101 macroporous resin has the best adsorption and desorption effect. Through the investigation on the dynamic parameters of adsorption and desorption of D-101macroporous resin, the optimal conditions was obtained, adsorption conditions: the Sample concentration of flavonoids 1.55 mg/mL, flow velocity 2 mL/min, Sample volume 100 mL, then distilled water to wash, desorption conditions: eluant concentration 70% ethanol, eluant volume 250 mL, flow velocity of eluant 1 mL/min. Under the optimal conditions, the content of flavonoids is raised from 20.10 % to 80.32 %, ratio of desorption reaches 91.08%, and the yield of total flavones is 68.25%. The flavonoids from Artemisia Annua L. reveale obvious antioxidant effect on oil and fat. The antioxidant activity of flavonoids from Artemisia Annua L. is superior to not only ascorbic acid but also citric acid on oil, and it is somewhat higher than that of citric acid but inferior to ascorbic acid on fat.
2013, 30(4).
Abstract:Using 2-hydroxy-5-nitrobenzaldehyde as starting compound, ten novel 8-aminobenzo[4,5]furo [3, 2-d]pyrimidine derivatives were synthesized through cyanation, esterification, cyclization and chlorization. Title compounds were fully characterized by 1H NMR, 13C NMR, IR, and MS. In addition, the reaction conditions were explored, and got optimized condition.
YANG Cui-ling , WEI Bo , WANG Xiao-liang , GAO Shu-ling , ZHANG Zhe
2013, 30(4).
Abstract:Palygorskite clays were treated by different concentration of hydrochloric acid and calcinated at different temperatures. The modified Palygorskite clays were characterized by XRD and TEM, which were used as adsorbents for removal of sodium lignosulfonate from aqueous solutions. The adsorption experiments showed that the modified palygorskite clays which was treated with the concentration of 1.0 mol/L hydrochloric acid at 60~70℃for 6 h had the best adsorption performance compared with raw palygorskite clays and the calcinated ones. The absorption processes follow pseudo-second order kinetic model very well and absorption isotherms fit Langmuir equation. The apparent maximum adsorption capacity was 93.97 mg/g. The results indicate that the adsorption process is exothermic.
2013, 30(4).
Abstract:A novel process of preparing 1H-tetrazole acetic acid was reported in this paper. Firstly, 5-amino tetrazole was synthesized in 85% yield from hydrazine hydrate and cyanamide. The second step was deamination reaction (the yield was 95%). The last step was nucleophilic substitution. Under basic condition, 1H-tetrazole acetic acid was produced by 1H-tetrazole and chloroacetic acid in 81.7% yield. Water was used as the reaction medium in the above steps. The total yield of 1H-tetrazole acetic acid was higher than 65%. In this paper, the most important work focused on the optimization of nucleophilic substitution. The better conditions for this substitution: reaction temperature 100 ℃, n(1H-tetrazole):n(ClCH2COOH):n(NaHCO3)=1:1:2.2, the reaction time 20 h.
ZHAO Yun , HU Mei-ling , JI xuan , ZHANG Peng , ZHANG Zhao
2013, 30(4):0-0.
Abstract:Using bromobenzene and cholesterol as starting materials, 2,4-diaminophenyl cholesteryl ether was synthesized by nitration, reduction and etherification reactions. The optimum reaction conditions of etherification were determined. The preferred reaction conditions are : n(2,4-dinitrobromobenzen):n(cholesterol)=1.55:1, w (NaOH)=50% , reacting for 3.5h at 25℃ with Toluene as solvent. The yield of 2,4-diaminophenyl cholesteryl ether (C) is 72%.The structures of all products were characterized by IR and 1H NMR spectra.
2013, 30(4):0-0.
Abstract:A asymmetric transfer hydrogenation to synthesize R-3,5-(trifluoro-dimethyl) benzene ethanol from 3,5-Bis(trifluoromethyl)acetophenone in isopropyl alcohol by using [RuCl2(C10H14)2]2 as catalyst and (1S, 2R) - (-) - 1 - amino - 2 - indene alcohol as ligands was discussed in this paper,reaction time 6h, reaction temperature 50℃, catalyst/ligands ratio 1:2.5, Substrate concentration 0.0957mol/L, The conversion rate of the product was 99%. Selective(ee) was 91.2% The target product was characterized by means of FTIR and 1H NMR.
Zhou Yu-han , GONG Run-jun , MIAO Wei-rong , Qu Jing-ping
2013, 30(4).
Abstract:Several new aromatic condensed-cyclic semicarbazone derivatives with the structure of indene were prepared from 4-chlorophenylacetic acid in 7%-9% yield, through cyclization, oxidation, condensation, hydrogenation, acylation etc.. Their structures were confirmed through 1H NMR and HRMS. Preliminary bioassay showed that most of them exhibited good activities toward various insects. Methyl 7-chloro-2,5-dihydro-2-[[(methoxycarbonyl)[4-(trifluoromethyl)- phenyl]amino]carbonyl] indeno[1,2-][1,3,4]oxadiazine-4a(3H)-carboxylate (12b) even shows higher activity than Indoxacarb.