地拉韦啶的合成及晶体结构

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(C₂₃H₃₂N₆O₄S), 并用核磁共振氢谱(¹H NMR)和核磁共振碳谱(¹³C 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=1.315 g/cm³, λ=0.071 073 nm, μ=0.172 mm^-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(Rint=0.040 7), 在I>2σ(I)时可观察到4 099个衍射点.

Synthesis and Crystal Structure of Delavirdine

The title compound delavirdine (C₂₃H₃₂N₆O₄S) 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. Itbelongs to the orthorhombic system, with space group P2₁2₁2₁ with 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=2.4685(15) nm³, Mr=488.61, Z=4, Dc=1.315 g/cm³, λ=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 I>2σ(I).