Synthesis and Crystal Structure of Mesityl Acetic Acid 3-Mesityl-2-oxo-1-oxaspiro[4,4]non-3-en-4-yl Ester  

作　　者：周勇 徐旭辉 程敬丽 朱国念 赵金浩 

机构地区：[1]Institute of Pesticide and Environmental Toxicology,Zhejiang University [2]College of Chemical Engineering and Materials Science,Zhejiang University of Technology

出　　处：《Chinese Journal of Structural Chemistry》2010年第4期515-518,共4页结构化学（英文）

基　　金：Supported by the Natural Science Foundation of Zhejiang Province (2008C21029)

摘　　要：The title compound mesityl acetic acid 3-mesityl-2-oxo-1-oxaspiro[4,4]non-3-en-4-yl ester （5, C28H32O4, Mr = 432.56）, as a spiromesifen derivative, has been synthesized by the conden- sation reaction of 2,4,6-trimethylphenylacetic chloride with 4-hydroxyl-3-mesityl-1-oxa-spiro[4,4]- non-3-en-2-one （4）, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9261（7）, b = 8.2802（8）, c = 18.7604（18） , α = 91.576（3）, β = 93.277（2）, γ = 95.306（12）o, V = 1223.3（2） 3, Z = 2, Dc = 1.174 g/cm3, F（000） = 464, μ = 0.077 mm–1, S = 1.001, the final R = 0.0624 and wR = 0.1415 for 2809 observed reflections with I 2σ（I） and 290 variable parameters. The crystal analysis results show that the five-membered cyclopentyl ring displays an envelope conformation with C（25） atom at the flap position, 0.537（3） out of the mean plane formed by the other four atoms. The dihedral angles between the two benzene and furan rings are 70.0（2） and 80.67（3）o, respectively.The title compound mesityl acetic acid 3-mesityl-2-oxo-1-oxaspiro[4,4]non-3-en-4-yl ester （5, C28H32O4, Mr = 432.56）, as a spiromesifen derivative, has been synthesized by the conden- sation reaction of 2,4,6-trimethylphenylacetic chloride with 4-hydroxyl-3-mesityl-1-oxa-spiro[4,4]- non-3-en-2-one （4）, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9261（7）, b = 8.2802（8）, c = 18.7604（18） , α = 91.576（3）, β = 93.277（2）, γ = 95.306（12）o, V = 1223.3（2） 3, Z = 2, Dc = 1.174 g/cm3, F（000） = 464, μ = 0.077 mm–1, S = 1.001, the final R = 0.0624 and wR = 0.1415 for 2809 observed reflections with I 2σ（I） and 290 variable parameters. The crystal analysis results show that the five-membered cyclopentyl ring displays an envelope conformation with C（25） atom at the flap position, 0.537（3） out of the mean plane formed by the other four atoms. The dihedral angles between the two benzene and furan rings are 70.0（2） and 80.67（3）o, respectively.

关 键 词：tetronic acids spiromesifen synthesis crystal structure 

分 类 号：O623.624[理学—有机化学]