《3,4-二乙酰基-2,5-已二酮的电化学合成及其晶体结构》.pdfVIP

人工晶体学报980121 人工晶体学报 科技期刊 JOURNAL OF SYNTHETIC CRYSTALS 1998年 第27卷 第1期 No1Vo27.1998 3,4-二乙酰基-2，5-已二酮的电化学合成 及其晶体结构* 朱洪友　杨宗璐　刘复初 •(云南大学化学系，昆明　650091) 郁开北 (中国科学院成都分院分析测试中心，成都　610041) 提要：以KI-NaI为电解质，丙酮为溶剂，用间接电氧化的方法对乙酰丙酮进行电解氧化偶联反应，高产率地得 1 到了3，4-二乙酰基-2，5-已二酮，用IR、UV、H NMR、高分辩质谱等对其进行了表征，并用X射线衍射测定 3 3 D =1.291×10 kg/m。XRD结果显示该分子完全以烯醇式存在，位于同一平面内，烯醇氢原子在分子内以不对 c 称形式与邻近的氧原子缔合。 关键词：间接电氧化，3，4-二乙酰基-2，5-已二酮，晶体结构，I /KI-NaI-丙酮，偶联 2 Electrochemical Synthesis and Crystal Structure of 3,4-Diacetyl-2,5-Hexanedione ** Zhu Hongyou　 Yang Zonglu　 Liu Fuchu　 Yu Kaibei (Department of Chemistry,Yunnan University,Kunming 650091,China) **(Chengdu Institute of Centre of Analysis and Determination,Chinese Academy of Sciences,Chengdu 610041,China) (Received 25 April 1997,accepted 8 December 1997) Abstract Indirect electrochemical coupling reaction of acetoacetone was studied using KI-NaI as the indirect electrolyte and acetone as solvent.The experimental results showed that this system afforded better yield for synthesis of 3,4-diacetyl- 2,5-hexanedione.The struture of the title compound was characteriazed by IR 、UV 、1H NMR 、high resolution MS, and also determined by X-ray diffraction analysis.The crystal is rhombic with space group Pbc