苏式三唑醇的晶体结构和波谱分析

Crystal structure and spectral analysis of threo-triadimenol

目的测定苏式三唑醇的物理常数、波谱数据、晶体结构参数,了解其结构和性质。方法测定苏式三唑醇的熔点、旋光度、紫外光谱、红外光谱、核磁共振、液质联用、X射线单晶衍射,并进行数据分析。结果苏式三唑醇的化学结构为dl-threo-1-(对氯苯氧基)-1-(1',2',4'-三氮唑-1'-基)-3,3-二甲基-2-丁醇。晶体属于斜方晶系,空间群为Pbca,a=9.5315(3),b=7.8690(5),c=39.919(2)?,V=2994.1(3)?~3,Z=8,Dc=1.312 g·cm^(-3),F(000)=1248,m=2.308 mm^(-1),R=0.0787,wR=0.2011。1R2S上的2'N与1S2R中2-OH的H形成氢键,同时1S2R的2'N与1R2S的2-OH的H形成氢键,相互连接形成晶体。进行了波谱数据的归属。结论苏式三唑醇由1R2S、1S2R的一对对映异构体以1∶1的比例存在,系首次报道。丰富了三唑醇的结构数据和理化性质。

Objective To determine the physical constants, spectra data, and single crystal diffraction and analyze the structure and property of threo-triadimenol. Methods The melting point, optical rotation, ultraviolet absorption spectrum, infrared absorption spectroscopy, nuclear magnetic resonance spectroscopy, liquid chromatography-mass spectrometry, and X-ray single crystal diffraction were determined and analyzed. Results The structure was dl-threo- 1-（p-chlorophenoxy）- 1-（1＇, 2＇, 4＇-triazole- 1＇-yl）-3, 3-dimethylbutanol-2. It was crystallized in the orthorhombic system, space group Pbca, a = 9.5315 （3）, b = 7.8690 （5）, c = 39.919 （2） A, V= 2994.1 （3） A3,Z= 8, De= 1.312g·cm 3, F（000）= 1248, m= 2.308mm-1,R= 0.0787, andwR= 0.2011. The hydrogen bonding structure of the crystal stacking was formed by 2＇N of 1R2S and H of 2-OH of 1S2R and 2＇N of 1S2R and H of 2-OH of 1R2S alternately. The spectral data were assigned. Conclusion Threo- triadimenol has been first reported to occur at the ratio of 1 ： 1 with a couple of enantiomers of IR2S and 1S2R. The structural data and physicochemical properties are enriched.