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A Convenient Synthesis of Acaricide Propargite

LIU Lin, XUE Shou-qing, QIAN Jian-hua, MA Cheng-xiang

Abstract （2005）

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2-(4-tert-butyl-phenoxy) cyclohexanol was synthesized through the reaction of 4-tert-butylphenol with epoxycyclohexane in the presence of catalyst, and through two steps of thionyl chloride derivatives alcoholysis, neutralization to produce propargite under condition of 15 ℃. 1NMR and IR were performed to determine the structure of intermediates and final product. The results show that the analytical sample is identical to authentic, and the chemical structure and the quality of this compound agreed with those of imported samples. Factors influencing the reaction yield were studied, such as feeding mode and reactions times. The optimum technical condition: 2-(4-tert-butyl-phenoxy) cyclohexanol is prepared from 4-tert-butylphenol and epoxycyclohexane and then thionyl chloride derivatives alcoholysis chlorinated sulfoxides to get intermediates. Intermediates reacted with propargyl alcohol in the presence of toluene to obtain the target material of 2-(4-tert-butyl-phenoxy) cyclohexanol. The total yield can be reach to 82% (based on 4-tert-butyl-phenol) and the purity is 98%.

2010, 23 (1): 47-49. DOI: 10.3696/j.issn.1006-396X.2010.01.012

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Reaction Property Research of Magnetic Loaded Nano-Catalyst to Synthesized Benzyl Butyrate

QIAN Jian-hua, QIN Jin-lan, LIU Lin, XING Jin-juan, TIAN Jing-bo

Abstract （287）

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Magnetic nano-Fe3O4 was prepared by hydrothermal method which was further to synthesis S2O2-8/Fe3O4, a magnetic nano-catalyst prepared by impregnation and ultrasonic method. Benzyl butyrate was catalytic synthesized with S2O2-8/Fe3O4, the influences of the loaded amount over the catalyst, activation temperature on the reaction were researched, and the recovery and reuse of the catalyst were discussed. The results indicate the esterification rate of the synthesized reaction by impregnation method is 85.6%, the purity of the product is 94.1%, while the selectivity of the catalyst obtained by ultrasonic method have an advantage over it obtained by impregnation method. 

2008, 21 (3): 43-45.

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The Synthesis of 1-Chloro-2,4,5-Trimethyl-Benzene

LIU Lin， XING Jin-juan， QIAN Jian-huan， ZHANG Qin-chun

Abstract （277）

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1-Chloro-2,4,5-trimethyl-benzene was synthesized by one-step method, unsym- trimethylbenzene as the raw material, while HCl-H ₂O ₂-CH ₃COOH as the catalytic activity system. By the orthorhombic experiment, the influenced factors are considered and the optimum conditions are confirmed. The experiment was carried under 60℃ for 2 h, while the mole ratio of H ₂O ₂ and unsym- trimethylbenzene is 4.5, HCl and unsym- trimethylbenzene is 4.0. The average yield was 82.8%, and the conversion rate was 98.4% while the fineness 99% under those conditions.

2008, 21 (2): 53-54.

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The Comprehensive Utilization of C ₉ Aromatic Hydrocarbons and Catalytic Synthesis of 2′,4′,6′-Trimethyl-2-Chloro-Acetophenone

QIAN Jian-hua，ZHANG Peng, XING Jin-juan,WANG Dao-lin, LIU Lin*

Abstract （279）

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2′,4′,6′-Trimethyl-2-chloro-acetophenone was catalytic synthesized from mesitylene which was obtained from by-product C ₉ aromatic hydrocarbons, the refinery and chloroacetyl chloride with Friedel-Crafts acylation reaction by metal loaded catalyst. The influencing factors in the reaction were studied by the contrastive experimental results. The results show that metal loaded catalyst has a better catalytic activity for the acylation reaction of mesitylene and chloroacetyl chloride. The study on optimization of reaction conditions indicates that the yield of acylation reaction at 80 ℃ was over 91.2% after 4 h when the mole ratio of chloroacetyl chloride and mesetylene to loaded metal catalyst was 2∶1∶0.002 5. The compound was identified by refractive index and IR spectrum.

2007, 20 (4): 10-12.

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A Novel Synthetic Method of 4-Chloro-1,2-Bimethyl-Benzene by High Selective Chlorination Reaction

QIAN Jian-hua, ZHANG Qing-chun, LIU Lin, XING Jin-juan, GONG Shu-hua

Abstract （142）

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The selective chlorination reaction of the aromatic ring among the aromatic compounds is very important in the economy and environmental protection aspects. A novel chlorination reaction system HCl-H₂O ₂-CH₃COOH was applied to react with o-xylene. Compared to the traditional Lewis acid catalysts which comprised sulfur and zeolite catalytic chlorination system, it took on much superiority such as high-selectivity, high-yield, simple operation, savings and environmental protection etc. The reaction conditions were controlled, the molar ratios of hydrogen peroxide, hydrochloric acid to o-xylene were 5.0,4.0 respectively, the reaction was processing under 70 ℃ until the feeding was finished and then the reaction was 2 h under 90 ℃. The conversion ratio of the raw material is over 99%, the yield is 96.9% and the selectivity is over 99% under this condition.

2007, 20 (1): 39-41.