Bis(2-benzimidazolyl)propane was synthesized by the reaction of o-phenylenediamine and glutaric acid which was accelerated by microwave irradiation and catalyzed by poly phosphoric acid(PPA) under solvent-free conditi...Bis(2-benzimidazolyl)propane was synthesized by the reaction of o-phenylenediamine and glutaric acid which was accelerated by microwave irradiation and catalyzed by poly phosphoric acid(PPA) under solvent-free condition. By the method of orthogonal experiment optimize synthesis factors which affect the reation: o-Phenylent Diamine: glutaric acid:2.2∶1.0(mol:mol),PPA:9.0g,time of microwave irradiation:8min, and the power of microwave irradiation:160W. Under the optimal condition, the highest yield of Bis(2-benzimidazolyl) propane is 77.4%. The products were characterized by melting point determination, IR spectrogram,1HNMR spectra and 13CNMR spectra.展开更多
3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Th...3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Thr with unprotected hydroxyl group on their side chain.Thus,DEPBT is useful for the synthesis of peptide alcohols,which have attracted much attention not only as the ligands but also as the enzyme inhibitors.A side reaction of DEPBT was found in the synthesis of Boc-β-Ala-HisOMe with unprotected imidazolyl group.In this paper,the discovery of this side reaction and the confirmation of the structure of this side product were reported.In addition,the influence of different reaction conditions on the side reaction were studied.Imidazolyl group was a key factor to cause the side reaction,excess DEPBT and high reaction temperature promoted the side reaction.展开更多
The dinuclear complexes [Zn（MIMHA）]2（MIMHAH=N-[（1-methylimidazole-2-yl）methyl]-β-alanine） was prepared and characterized by single-crystal X-ray analysis.Crystal data:monlclineic,space group P21/c,a=8.792（2）,...The dinuclear complexes [Zn（MIMHA）]2（MIMHAH=N-[（1-methylimidazole-2-yl）methyl]-β-alanine） was prepared and characterized by single-crystal X-ray analysis.Crystal data:monlclineic,space group P21/c,a=8.792（2）,b=9.267（2）,c=16.942（2）?,β=99.5（2）,V=1351.6（2）?3,and Z=2.The zinc（Ⅱ） atom was co-ordinated in a tetrahedral geometry（N2Cl2）,which positions were occupied by one nitrogen atom and one oxygen atom from the ligand and two chlorine atoms.展开更多
文摘Bis(2-benzimidazolyl)propane was synthesized by the reaction of o-phenylenediamine and glutaric acid which was accelerated by microwave irradiation and catalyzed by poly phosphoric acid(PPA) under solvent-free condition. By the method of orthogonal experiment optimize synthesis factors which affect the reation: o-Phenylent Diamine: glutaric acid:2.2∶1.0(mol:mol),PPA:9.0g,time of microwave irradiation:8min, and the power of microwave irradiation:160W. Under the optimal condition, the highest yield of Bis(2-benzimidazolyl) propane is 77.4%. The products were characterized by melting point determination, IR spectrogram,1HNMR spectra and 13CNMR spectra.
文摘3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Thr with unprotected hydroxyl group on their side chain.Thus,DEPBT is useful for the synthesis of peptide alcohols,which have attracted much attention not only as the ligands but also as the enzyme inhibitors.A side reaction of DEPBT was found in the synthesis of Boc-β-Ala-HisOMe with unprotected imidazolyl group.In this paper,the discovery of this side reaction and the confirmation of the structure of this side product were reported.In addition,the influence of different reaction conditions on the side reaction were studied.Imidazolyl group was a key factor to cause the side reaction,excess DEPBT and high reaction temperature promoted the side reaction.
文摘The dinuclear complexes [Zn（MIMHA）]2（MIMHAH=N-[（1-methylimidazole-2-yl）methyl]-β-alanine） was prepared and characterized by single-crystal X-ray analysis.Crystal data:monlclineic,space group P21/c,a=8.792（2）,b=9.267（2）,c=16.942（2）?,β=99.5（2）,V=1351.6（2）?3,and Z=2.The zinc（Ⅱ） atom was co-ordinated in a tetrahedral geometry（N2Cl2）,which positions were occupied by one nitrogen atom and one oxygen atom from the ligand and two chlorine atoms.
基金The project was supported by the National Natural Science Foundation of China(2130609221476133)+1 种基金Science and Technology Plan Project of Shandong Provincial UniversityChina(J12LA02)~~
