螯形主体分子的设计、包结性能及其在细辛挥发油 有效成分选择分离中的应用

设计了两种新的具有螯形骨架的主体分子反式-1,2-二苯基-1,2-苊二醇(1)和顺式-1,2-二(1'-萘基)-1,2-苊二醇(2)，主体(1)，(2)可与许多有机小分子化合物形成配位包合物。用IR和粉末XRD表征了主体分子(1)和(2)的包结物，用^1NMR测定了包结物的主客体分子摩尔比：(1)·DMF(1:2)，(1)·DMSO(1:2)，(1)·THF(1:2)，(1)·二氧六环(1:1)，(1)·吡啶(1:1)，(2)·DMF(1:1)和(2)·DMSO(1:1)。单晶X射线衍射分析了包结物的晶体结构，(1)·DMF：空间群Pnaa，a=0.9377(1)nm，b=1.4351(1)nm，c=4.0463(3)nm；(1)·DMSO：空间群Pbcn，a=1.6278(1)nm，b=1.0751(1)nm，c=1.4980(1)nm；(2)·DMF：P2~1/n，a=0.9796(1)nm，b=1.2377(1)nm，c=2.2344(3)nm，β=93.02(1)°；游离主体(1)：空间群P1，a=1.0461(1)nm，b=1.1213(1)nm，c=1.5496(1)nm，α=81.74(1)°，β=75.71(1)°，γ=89.00(1)°；分析了主体分子的刚性和柔韧性对包结性能的影响。并研究了主体分子(1)选择分离细辛挥发油，将顺甲基异丁香酚从挥发油中分离出来。

Design of chela-shaped clathrate hosts, inclusion properties and its application of selective isolation of effective component from volatile oil of Chinese herb xixin

Two new clathrate hosts characteristic of a chela-shaped molecular back bone, trans-1,2-biphenyl-1,2-acenaphthenodiol 1 and cis-1,2-bi- 1'-naphthyl-1,2-acenaphthenediol 2 were designed. 1 and 2 can form coordinatoclanthrate with various small organic compounds and these inclusion compounds were confirmed by means of IR and powder XRD. The host-go\uest molar ratios were determined by ^1H NMR and the following results were found: (1)·DMF(1 : 2), (1)·DMSO(1 : 2), (1) ·THF(1 : 2), (1)·1,4-dioxane(1 : 1), 1·pyridine(1 : 1), (2)·DMF(1 : 1) and (2)·DMSO(1 : 1). The single crystal structures of new inclusion compounds were determined by X-ray diffraction analysis. The crystal of host(1)·DMF belongs to space group Pnaa, a=0.9377(1) nm, b=1.4351(1) nm, c=4.0463(3) nm and 1·DMSO has space group Pbcn, a=1.6278(1) nm, b=1.0751(1) nm, c=1.4980(1) nm and host(2)·DMF belongs to P2~1/n，a=0.9796(1) nm, b=1.2377(1) nm, c=2.2344(3) nm, β =93.02(1)°. The crystal analysis of freehost (1) showed space group P1, and a=1.0461(1) nm, b=1.1213(1) nm, c=1.5496(1) nm, α=81.74(1)°, β=75.71(1)°, γ=89.00(1)°. The effect of rigidity and flexibility of host molecules on inclusion properties were discussed. The selective isolation of the effective component (1,2-dimethoxy-4-2'- propenylbenzene) from the volatile oil of Chinese herb Xixin by host(1) was carried out.