地拉韦啶的合成及晶体结构

Synthesis and Crystal Structure of Delavirdine

以烟酰胺、对硝基苯肼和丙酮酸乙酯等为原料合成目标化合物地拉韦啶(C23H32N6O4S),并用核磁共振氢谱(1 H NMR)和核磁共振碳谱(13 C NMR)表征其结构,通过X射线单晶衍射确定其晶体结构.实验结果表明:该晶体属于正交晶系,P212121空间群;晶体学数据为:a=1.096 9(4)nm,b=1.152 5(4)nm,c=1.951 0(7)nm,α=90°,β=90°,γ=90°,V=2.468 5(15)nm3,Mr=488.61,Z=4,Dc=1.315g/cm3,λ=0.071 073nm,μ=0.172mm-1,F(000)=1 040,R=0.040 7,wR=0.090 5;共收集14 875个衍射点,其中4 851个为独立衍射点(Rint=0.040 7),在I>2σ(I)时可观察到4 099个衍射点.

The title compound delavirdine （C23 H32N6O4S） has been synthesized from nicotinamide,4-nitrophenylhydrazine and ethyl pyruvate. It was characterized by means of 1H NMR and 13C NMR. Its crystal and molecular structures were determined by X-ray diffractometry. It belongs to theorthorhombicsystem, with space group P212121 with a= 1. 096 9（4）nm, b= 1. 152 5（4）nm; c=1.9510（7）nm, α = 90°, β= 90°, γ= 90°, V= 2. 468 5 （15） nm3, Mr= 488. 61, Z= 4,Dc=1.315 g/cm3, ）.=0.071 073 nm, μ=0. 172 mm-1, F（000）=1 040, the final R=0. 040 7 and wR=0.090 5. A total of 14 875 reflections were collected, of which 4 851 were independent（Rint=0. 040 7） and 4 099 were observed with γ.