多取代茚并[1,2-d]哒嗪的合成和结构表征

Synthesis and Crystal Structure of Polysubstituted Indeno[1,2-d]Pyridazines

标题化合物C38.50H32Cl2N2O4S2是由3-(2-(对氯苯基乙炔基)苯基)-1-(对甲苯基)丙-2-烯-1-酮、对甲苯磺酰肼在室温的空气条件下使用TBHP/I2系统,在乙腈(CH3CN)作为溶剂中反应得到。通过单晶X射线衍射法测定结构,其晶体属三斜晶系,空间群P-1,a=1.15045(9)nm,b=1.18251(10)nm,c=1.31168(12)nm,α=95.8450(10)°,β=101.153(2)°,γ=92.9430(10)°,V=1.7370(3)nm3,相对分子质量Mr=721.68,晶胞密度Dc=1.380g/cm^3,Z=2,λ=0.071073nm,吸收系数μ(MoKα)=0.351mm^-1,F(000)=750,最终偏离因子R=0.0802,wR=0.1783,S=1.003,(△/σ)max=0.001,(△ρ)min=323e/nm3和(△ρ)max=-463e/nm^3。文中分析了新形成的哒嗪环为船式构象。苯环(C11-C16)和哒嗪环基本是平行的,茚环上的五元环接近共面。

The title compound(C38.50H32Cl2N2O4S2)was synthesized by the reaction of 3-(2-(phenylethynyl)phenyl)-1-(p-tolyl)prop-2-en-1-one,P-toluenesulfonyl in acetonitrile(CH 3CN)under air conditions at room temperature using TBHP/I 2 system.Its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of Triclinic,space group P-1,a=1.15045(9)nm,b=1.18251(10)nm,c=1.31168(12)nm,α=95.8450(10)°,β=101.153(2)°,γ=92.9430(10)°,V=1.7370(3)nm 3,M r=721.68,Z=2,D c=1.380 g/cm 3,μ(MoKα)=0.351 mm-1,F(000)=750,the final R=0.0802 and wR=0.1783,S=1.003,(△/σ)max=0.001,(△ρ)min=323 e/nm 3 and(△ρ)max=-463 e/nm 3.The newly formed pyridazine ring is analyzed as a ship-like conformation.The benzene ring(C11-C16)and the azine ring are substantially parallel and the five-membered ring on the indeno ring is close to coplanar.