摘要
标题化合物C14H12N2在无溶剂条件下,用微波辐射法以盐酸作催化剂、邻苯二胺和苯乙酸为原料合成得到。最优化的合成条件是:n(邻苯二胺)∶n(苯乙酸)=1∶1.2(即邻苯二胺1.08 g,苯乙酸1.63 g),盐酸用量2mL,辐射时间8 min,微波功率480 W。用IR、1HNMR对产物进行了表征,并用单晶X射线衍射法测定了其单晶结构,标题化合物晶体属正交晶系,空间群Pbca,Mr=208.26,a=9.384 2(13)nm,b=9.723 4(13)nm,c=2.493 7(3)nm,V=2.275 4(5)nm3,Z=8,Dc=1.216 g/cm3,F(000)=880,μ=0.073 mm-1,GOF=1.001,R1=0.042 6,wR2=0.097 6〔Ⅰ>2σ(Ⅰ)〕。
2-Phenylbenzimidazole（ Ⅰ ） was synthesized by solvent-free reaction of o-phenylenediamine （ Ⅱ ） and phenylaeetie acid （Ⅲ ） accelerated by microwave irradiation and catalyzed by HCl. The optimal reaction conditions were ： n （ Ⅱ） ： n （ Ⅲ ） = 1 ： 1.2 （ Ⅱ 1.08 g, Ⅲ 1.63 g）, HCl 2 mL, time of microwave irradiation 8 min and microwave power 460 W. The product was characterized by IR and ^1HNMR spectra, and its crystal structure was determined by X-ray single crystal diffraction. Ⅰ belongs to orthorhombie system with space group Pbea ,Mr = 208.26, a = 9. 384 2 （ 13 ） nm, b = 9. 723 4 （ 13 ） nm,c=2.493 7（3） nm, V=2.275 4（5） nm^3,Z=8,Dc =1.216 g/cm^3,F（000） =880, =0.073 mm^-1,GOF=1.001,R1=0.042 6,wR2 =0.097 6[ I 〉2σ（ I ）1.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2008年第2期121-124,共4页
Fine Chemicals
关键词
苯并咪唑
邻苯二胺
晶体结构
微波辐射
功能材料
benzimidazole
o-phenylenediamine
crystal structure
microwave irradiation
functional materials
