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目的 利用分子设计 ,合成新型大环多胺配体BDBPH ,研究其合成工艺及晶体结构。方法 2 ,6 二甲酰基对甲苯酚 ,二亚乙基三胺 ,Pb(SCN) 2 三种化合物在CHCl3溶液中 50～ 6 0℃反应 18h ,随后经NaBH4 还原、脱Pb2 + 等操作 ,得晶体产品BDBPH ,用1HNMR、FAB—MS、元素分析确定了其结构 ,用单晶X 射线衍射法测定其晶体结构。结果 1HNMR(D2 O) ,δ(ppm) :2 .13(s , CH3,6H) ,3.35(q ,ethylene ,16H) ,4 .2 1(s , CH2 ,8H) ,7.16 (s ,Ary1,4H) ;FAB MS :4 71(M +H ) ;元素分析 ,计算值 (BDBPH·6HBr·4H2 O) :C 30 .35,H 5.4 4 ,N 8.17,实测值 :C 30 .2 2 ,H 5.4 6 ,N7.98。晶体属单斜晶系 ,P2 1/C空间群 ,晶体学参数 :a =14.4 4 1(5) ,b =11.4 82 (4 ) ,c =12 .0 90 (6 ) ,α =90 ,β =96 .92 (3) ,γ =90℃ ,V =1990 .0 (14) 3。大环分子采取椅式构型 ,6个Br- ,4个H2 O分子对称分布于大环两侧。结论 该大环配体合成工艺先进 ,晶体结构新颖 ,可用于多种金属配合物的研究 ,对进一步了解金属酶的结构及其催化作用机制具有重要意义。
OBJECTIVE To synthesize new macrocyclic polyamine ligand BDBPH by molecular design and study its synthesis process and crystal structure. Method 2, 6 Two formyl p-cresol, diethylenetriamine, Pb (SCN) 2 three kinds of compounds in CHCl3 solution 50 ~ 6 0 ℃ reaction 18h, followed by NaBH4 reduction, Pb2 + and other operations were The crystal structure of BDBPH was confirmed by 1HNMR, FAB-MS and elemental analysis. The crystal structure was determined by single crystal X-ray diffraction. Results 1HNMR (D2 O), δ (ppm): 2.13 (s, CH3, 6H), 3.35 (q, ethylene, 16H), 4.21 (s, 4H); FAB MS: 4171 (M + H); Anal. Calcd. For (BDBPH.6HBr.4H2O): C30.35, H 5.44, N 8.17, Found: C30.22, H 5.4 6, N7.98. The crystal is a monoclinic, P2 1 / C space group with crystallographic parameters of a = 14.4 4 1 (5), b = 11.4 82 (4), c = 12.090 (6), α = 90, β = 96.92 (3), γ = 90 ° C, V = 1990.0 (14) 3. Macrocyclic molecules take the chair-type configuration, 6 Br-, 4 H2 O molecules symmetrically distributed on both sides of the ring. CONCLUSION The macrocyclic ligand has advanced synthesis technology, novel crystal structure and can be used for the study of various metal complexes. It is of great significance to further understand the structure of the metalloenzyme and its catalytic mechanism.