Synthesis and Crystal Structure of 12-(2,4-Dichlorophenyl)-7,8,9,10,11,12-hexahydrobenzo[f]pyrimido [4,5-b]quinoline-9,11-dione DMF Solvate  

作　　者：王香善 李庆 吴健蓉 张梅梅 

机构地区：[1]School of Chemistry and Chemical Engineering,Xuzhou Normal University [2]Key Laboratory of Biotechnology for Medical Plant,Xuzhou Normal University

出　　处：《Chinese Journal of Structural Chemistry》2010年第3期335-340,共6页结构化学（英文）

基　　金：Supported by the National Natural Science Foundation of China (20802061);the Natural Science Foundation (08KJD150019);Qinglan Project (08QLT001) of Jiangsu Education Committee

摘　　要：The title compound 12-（2,4-dichlorophenyl）-7,8,9,10,11,12-hexahydrobenzo-[f]pyrimido[4,5-b]quinoline-9,11-dione DMF solvate 1（C24H20Cl2N4O3,Mr=483.34） was synthesized and crystallized.The crystal belongs to the monoclinic system,space group P21/n with a=6.4798（16）,b=20.595（5）,c=16.723（4）,β=95.267（7）o,Z=4,V=2222.3（9）3,Dc=1.445 g/cm3,μ（MoKα）=0.328 mm-1,F（000）=1000,the final R=0.0530 and wR=0.1388 for 3484 observed reflections（I2σ（I））.X-ray analysis reveals that the central 1,4-dihydropyridine ring is slightly distorted,adopting a half-chair conformation,which is obviously different from the boat conformations of other similar compounds.In addition,the classical hydrogen bonds of N（2）-H（2A）…O（2） are presented in the crystals,and link the adjacent molecules to form dimmers.Atom O（3） in the DMF solvent forms two hydrogen bonds of O（3）…H（1H）-N（1） and O（3）…H（3H）-N（3） with a pyrimidoquinoline moiety,forming an interesting half-chair-like conformation.The hydrogen bonds link the molecules to form dimmers,while intermolecular π-π interaction connects the above-mentioned dimmers to yield a one-dimensional structure.The title compound 12-（2,4-dichlorophenyl）-7,8,9,10,11,12-hexahydrobenzo-[f]pyrimido[4,5-b]quinoline-9,11-dione DMF solvate 1（C24H20Cl2N4O3,Mr=483.34） was synthesized and crystallized.The crystal belongs to the monoclinic system,space group P21/n with a=6.4798（16）,b=20.595（5）,c=16.723（4）,β=95.267（7）o,Z=4,V=2222.3（9）3,Dc=1.445 g/cm3,μ（MoKα）=0.328 mm-1,F（000）=1000,the final R=0.0530 and wR=0.1388 for 3484 observed reflections（I2σ（I））.X-ray analysis reveals that the central 1,4-dihydropyridine ring is slightly distorted,adopting a half-chair conformation,which is obviously different from the boat conformations of other similar compounds.In addition,the classical hydrogen bonds of N（2）-H（2A）…O（2） are presented in the crystals,and link the adjacent molecules to form dimmers.Atom O（3） in the DMF solvent forms two hydrogen bonds of O（3）…H（1H）-N（1） and O（3）…H（3H）-N（3） with a pyrimidoquinoline moiety,forming an interesting half-chair-like conformation.The hydrogen bonds link the molecules to form dimmers,while intermolecular π-π interaction connects the above-mentioned dimmers to yield a one-dimensional structure.

关 键 词：crystal structure pyrimidoquinoline synthesis 

分 类 号：O626.323[理学—有机化学]