4-溴-2-(溴甲基)苯甲醛是合成1,2-二氢酞嗪化合物的重要中间体。以4-溴-2-甲基苯腈为原料,通过溴代、还原得两步反应得到目标化合物4-溴-2-(溴甲基)苯甲醛。确定了溴代反应最佳条件:N-溴代丁二酰亚胺(24.0mmol)、过氧苯甲酰(4.0mmol),...4-溴-2-(溴甲基)苯甲醛是合成1,2-二氢酞嗪化合物的重要中间体。以4-溴-2-甲基苯腈为原料,通过溴代、还原得两步反应得到目标化合物4-溴-2-(溴甲基)苯甲醛。确定了溴代反应最佳条件:N-溴代丁二酰亚胺(24.0mmol)、过氧苯甲酰(4.0mmol),反应体系在CCl4中回流反应8h。还原反应最佳条件:二异丁基氢化铝(DIBAL-H)(12.0mmol),反应溶剂二氯甲烷,室温反应3h。两步反应总收率85.4%,产物及中间体结构通过1 H NMR、13 C NMR和电喷雾电离质谱(ESI-MS)进行了表征。展开更多
Title compounds have been synthesized.The structures and properties are determined by elemental analysis,UV Vis,IR spectrum,fluorescence spectrum,polarizing microscope.The synthetic conditions of porphyrin derivatives...Title compounds have been synthesized.The structures and properties are determined by elemental analysis,UV Vis,IR spectrum,fluorescence spectrum,polarizing microscope.The synthetic conditions of porphyrin derivatives and their properties,UV Vis,fluorescence spectrum are discussed briefly.展开更多
2-Bromo-4-methylphenol was synthesized from 4-methylphenol by oxidative bromination at the low temperature,with a yield of 93%.The product was characterized by IR and （）1H NMR spectroscopy.The optimum conditions of ...2-Bromo-4-methylphenol was synthesized from 4-methylphenol by oxidative bromination at the low temperature,with a yield of 93%.The product was characterized by IR and （）1H NMR spectroscopy.The optimum conditions of the reaction were:reaction temperature was-5～-10℃,the mol ratio of C7H8O:H2O2 was 1:0.85,reaction time was 4h and agitation rate was 1000 r/min.展开更多
文摘4-溴-2-(溴甲基)苯甲醛是合成1,2-二氢酞嗪化合物的重要中间体。以4-溴-2-甲基苯腈为原料,通过溴代、还原得两步反应得到目标化合物4-溴-2-(溴甲基)苯甲醛。确定了溴代反应最佳条件:N-溴代丁二酰亚胺(24.0mmol)、过氧苯甲酰(4.0mmol),反应体系在CCl4中回流反应8h。还原反应最佳条件:二异丁基氢化铝(DIBAL-H)(12.0mmol),反应溶剂二氯甲烷,室温反应3h。两步反应总收率85.4%,产物及中间体结构通过1 H NMR、13 C NMR和电喷雾电离质谱(ESI-MS)进行了表征。
文摘Title compounds have been synthesized.The structures and properties are determined by elemental analysis,UV Vis,IR spectrum,fluorescence spectrum,polarizing microscope.The synthetic conditions of porphyrin derivatives and their properties,UV Vis,fluorescence spectrum are discussed briefly.
文摘2-Bromo-4-methylphenol was synthesized from 4-methylphenol by oxidative bromination at the low temperature,with a yield of 93%.The product was characterized by IR and （）1H NMR spectroscopy.The optimum conditions of the reaction were:reaction temperature was-5～-10℃,the mol ratio of C7H8O:H2O2 was 1:0.85,reaction time was 4h and agitation rate was 1000 r/min.
