机构地区: 深圳大学化学与化工学院
出 处: 《精细化工》 2010年第3期260-263,共4页
摘 要: 以邻苯二胺、环己酮为原料,在微波辐射下合成得到标题化合物2-环己烷基-1,3-二氢苯并咪唑(C12H16N2,Mr=187.26),其合成条件是:n(邻苯二胺)∶n(环己酮)=1∶1.2(邻苯二胺1.08 g,环己酮1.18 g),冰醋酸2 mL,辐射时间3 min,微波功率153 W。用红外光谱和核磁共振氢谱对产物进行了表征,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Fdd2,a=2.060 0(4)nm,b=2.433 0(5)nm,c=0.855 00(17)nm,α=90°,β=90°,γ=90°,V=4.285 2(15)nm3,Z=16,Dc=1.161 g/m3,μ=0.070 mm-1,F(000)=1 616,GOF=1.002,R1=0.058 5,wR2=0.150 9。 The 2-cyclohexane-1,3-dihydro-benzimidazole(Ⅰ) was synthesized by the reaction of o-phenylenediamine(Ⅱ) and cyclohexanone(Ⅲ) accelerated by microwave irradiation and catalyzed by acetic acid.The optimal conditions are as follows:n(Ⅱ)∶n(Ⅲ)=1∶1.2(Ⅱ1.08 g,Ⅲ 1.18 g),acetic acid 2 mL,time of microwave irradiation 3 min,and microwave power 153 W.The product was characterized by IR and ^1HNMR spectra,and its crystal structure was determined by X-ray single crystal diffraction.The title compound 2-cyclohexane-1,3-dihydro-benzimidazole(C12H16N2,Mr=187.26) has been synthesized under microwave irradiation and the characterization was determined by single-crystal X-ray diffraction analysis.It crystallizes in orthorhombic,space group Fdd2 with a=2.060 0(4) nm,b=2.433 0(5) nm,c=0.855 00(17) nm,α=90°,β=90°,γ=90°,V=4.285 2(15) nm^3,Z=16,Dc=1.161 g/m3,μ=0.070 mm^-1,F(000)=1 616,GOF=1.002,R1=0.058 5,wR2=0.150 9.