分化诱导剂PMDH的合成及晶体结构

Synthesis and Crystal Structures of Cancer Cell Inducers of Differentiation PMDH

合成了分化诱导剂1,5-二[3,3’-（5,5-二甲基乙内酰脲）]戊烷（PMDH）,对合成方法和路线进行了优化,并通过元素分析。质谱、核磁和红外进行了表征.利用单晶X时线衍射仪测定了化合物的晶体结构,晶体属于三斜晶系,空间群为P1,晶体学参数为:α=0.874（4）nm,b=1.1146（2）nm,c=1.720（3）nm,α=87.20（3）°,β=89.77（3）°,γ=85.12（3）°,V=1.6686（6）nm,Z=4.最终偏离因子R1=0.0651.分子中的碳链连接两个乙内酰脲五元环,五元环与和它相连的两个碳基氧原子呈平面结构,分子间存在较强的氢键.

The effective inducer of differentiation, 3, 3'-(pentane-1, 5-diyl)bis(5, 5-dimethylhydantoin) (PMDH), was synthesized and identified by MS, NMR , IR and element analysis. Its synthetic method and route were optimized. The structure of the compound was determined by single crystal X-ray diffraction and compared with other Hexamethylenbisamide(HMBA) derivatives. The crystal structure of PMDH belongs to triclinic space group P 1. Crystallographic data are:α= 0. 874 1(4)nm, b =1.114 6(2) nm, c=1.721 °(3) nm;α= 87.20(3)°, B=89. 77(3)°, r=85.12(3)°, V=1.6686(6)nm3, DC=1.291g.cm-3,Z=4, F(000)=696, u=0. 095 mm-1, R1=0. 065l(for observed data), wR2=0.165 7(for unique data), S= 1. 08 1. The hyndantoin rings are planar. The molecules are linked by intermolecular hydrogen bonds to form infinite one-dimensional molecular chain almost parallel to the b axis.