The title complex [Sm(o-MOBA)3(phen)·H2O]2·4H2O has been synthesized by the reaction of SmCl3·6H2O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was de...The title complex [Sm(o-MOBA)3(phen)·H2O]2·4H2O has been synthesized by the reaction of SmCl3·6H2O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm3+ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.展开更多
研究了以1,10-邻菲罗啉为原料,经氧化和氯代反应合成2-氯-1,10-邻菲罗啉,再经氨基化反应得到目标产物2-氨基-1,10-邻菲罗啉,化合物结构经核磁共振仪、红外分光光度计和质谱仪确认。结果表明,氯代反应的优化反应条件:投料比为1 g:2 m L,...研究了以1,10-邻菲罗啉为原料,经氧化和氯代反应合成2-氯-1,10-邻菲罗啉,再经氨基化反应得到目标产物2-氨基-1,10-邻菲罗啉,化合物结构经核磁共振仪、红外分光光度计和质谱仪确认。结果表明,氯代反应的优化反应条件:投料比为1 g:2 m L,溶剂DMF用量为15 m L,反应时间为8 h;氨基化反应的优化反应条件:投料质量比为1:6,反应温度为180℃、时间为2.0 h。该工艺具有原料易得、工艺简单、环境友好等特点,为2-氨基-1,10-邻菲罗啉的合成提供了一条简便的合成路线。展开更多
采用Pd/C催化水合肼还原法制备了5-氨基-1,10-邻菲罗啉,利用IR,1 H NMR,MS和元素分析确认其结构.讨论了反应温度、反应时间、催化剂及还原剂用量对产物产率的影响.优化实验结果表明,5-氨基-1,10-邻菲罗啉的产率可达92.9%.Pd/C催化水合...采用Pd/C催化水合肼还原法制备了5-氨基-1,10-邻菲罗啉,利用IR,1 H NMR,MS和元素分析确认其结构.讨论了反应温度、反应时间、催化剂及还原剂用量对产物产率的影响.优化实验结果表明,5-氨基-1,10-邻菲罗啉的产率可达92.9%.Pd/C催化水合肼还原法是一种对环境友好、简单易行的加氢还原方法.展开更多
文摘The title complex [Sm(o-MOBA)3(phen)·H2O]2·4H2O has been synthesized by the reaction of SmCl3·6H2O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm3+ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.
文摘研究了以1,10-邻菲罗啉为原料,经氧化和氯代反应合成2-氯-1,10-邻菲罗啉,再经氨基化反应得到目标产物2-氨基-1,10-邻菲罗啉,化合物结构经核磁共振仪、红外分光光度计和质谱仪确认。结果表明,氯代反应的优化反应条件:投料比为1 g:2 m L,溶剂DMF用量为15 m L,反应时间为8 h;氨基化反应的优化反应条件:投料质量比为1:6,反应温度为180℃、时间为2.0 h。该工艺具有原料易得、工艺简单、环境友好等特点,为2-氨基-1,10-邻菲罗啉的合成提供了一条简便的合成路线。
文摘采用Pd/C催化水合肼还原法制备了5-氨基-1,10-邻菲罗啉,利用IR,1 H NMR,MS和元素分析确认其结构.讨论了反应温度、反应时间、催化剂及还原剂用量对产物产率的影响.优化实验结果表明,5-氨基-1,10-邻菲罗啉的产率可达92.9%.Pd/C催化水合肼还原法是一种对环境友好、简单易行的加氢还原方法.
