Six palladium? complexes with isonitrosoethylacetoacetate imine Schiff base ligands, Pd(R IEAI)2, were prepared and characterized by IR, Raman and electronic spectra. Complex tran Pd(p CH3C6H4 IEAI)2 (2) cry stallizes...Six palladium? complexes with isonitrosoethylacetoacetate imine Schiff base ligands, Pd(R IEAI)2, were prepared and characterized by IR, Raman and electronic spectra. Complex tran Pd(p CH3C6H4 IEAI)2 (2) cry stallizes in the monoclinic system, space group P21/c,with a=1.2002(2),b=0.9972(2),c=1.1121(2)nm,β=90.43(3)°,Z=2,F(000)=616,μ=7.44cm-1. The final R and wR are 0.0244 and 0.0625 for 2620 observed reflections with I ≥ 2σ(I), respectively. The geometry around the Pd? ions in those complexes has a distorted PdN4 square plane, the Schiff base ligands R IEAI- being coordinated through their oximino nitrogen atoms and imino nitrogen atoms.展开更多
以四乙酰基二苄基六氮杂异伍兹烷为基质,经亚硝解脱苄合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW);用纯硝酸氧化TADNSIW制备四乙酰基二硝基六氮杂异伍兹烷(TADNIW),收率93.0%,以上两步反应均在室温下完成。在85℃条件下,TADNIW经硝...以四乙酰基二苄基六氮杂异伍兹烷为基质,经亚硝解脱苄合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW);用纯硝酸氧化TADNSIW制备四乙酰基二硝基六氮杂异伍兹烷(TADNIW),收率93.0%,以上两步反应均在室温下完成。在85℃条件下,TADNIW经硝硫混酸硝解合成了六硝基六氮杂异伍兹烷(HNIW),反应时间50 m in,收率95.1%,质量分数98.80%。用硝硫混酸对TADNSIW进行硝解合成了HNIW,并优化了反应条件,反应温度90℃,反应时间60 m in,硝解剂必须大于14 mL(底物TADNSIW 1.2 g),收率为96.1%,质量分数98.87%。分别用FTIR,1HNMR和元素分析对目标化合物进行了表征。前体TADNSIW和TADNIW分子中只有乙酰基和亚硝基,它们的硝解反应体系较简单,反应时间短、反应条件温和,母液中只含有乙酸和硝解剂,产物易分离。展开更多
文摘Six palladium? complexes with isonitrosoethylacetoacetate imine Schiff base ligands, Pd(R IEAI)2, were prepared and characterized by IR, Raman and electronic spectra. Complex tran Pd(p CH3C6H4 IEAI)2 (2) cry stallizes in the monoclinic system, space group P21/c,with a=1.2002(2),b=0.9972(2),c=1.1121(2)nm,β=90.43(3)°,Z=2,F(000)=616,μ=7.44cm-1. The final R and wR are 0.0244 and 0.0625 for 2620 observed reflections with I ≥ 2σ(I), respectively. The geometry around the Pd? ions in those complexes has a distorted PdN4 square plane, the Schiff base ligands R IEAI- being coordinated through their oximino nitrogen atoms and imino nitrogen atoms.
文摘以四乙酰基二苄基六氮杂异伍兹烷为基质,经亚硝解脱苄合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW);用纯硝酸氧化TADNSIW制备四乙酰基二硝基六氮杂异伍兹烷(TADNIW),收率93.0%,以上两步反应均在室温下完成。在85℃条件下,TADNIW经硝硫混酸硝解合成了六硝基六氮杂异伍兹烷(HNIW),反应时间50 m in,收率95.1%,质量分数98.80%。用硝硫混酸对TADNSIW进行硝解合成了HNIW,并优化了反应条件,反应温度90℃,反应时间60 m in,硝解剂必须大于14 mL(底物TADNSIW 1.2 g),收率为96.1%,质量分数98.87%。分别用FTIR,1HNMR和元素分析对目标化合物进行了表征。前体TADNSIW和TADNIW分子中只有乙酰基和亚硝基,它们的硝解反应体系较简单,反应时间短、反应条件温和,母液中只含有乙酸和硝解剂,产物易分离。
