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 

作者机构：Institute of Pesticide and Environmental ToxicologyZhejiang University College of Chemical Engineering and Materials ScienceZhejiang University of Technology 

出 版 物：《Chinese Journal of Structural Chemistry》 (结构化学（英文）)

年 卷 期：2010年第29卷第4期

页      面：515-518页

核心收录：

学科分类：081704[工学-应用化学] 07[理学] 08[工学] 0817[工学-化学工程与技术] 070303[理学-有机化学] 0703[理学-化学] 

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

主　　题：tetronic acids spiromesifen synthesis crystal structure 

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.