【摘要】 以苯酐和尿素为原料,经过脱水环化、混酸硝化、Fe粉还原制备4-氨基邻苯二甲酰亚胺.在脱水环化反应中,加入催化剂以及甲苯作为脱水剂,回流蒸出生成的水分,缩短了反应时间,收率达到98.0%;在硝化反应中,加入P2O5作为吸水剂,使浓H2SO4的用量减少一半,收率高于80.0%;在还原反应中,加入NH4C l作为电解质,滴加浓HC l,调节pH至4~5,使Fe粉活化更充分,收率达到91.1%.目标产物用差示描扫(DSC)和红外光谱进行表征.实验结果表明:产物的熔点为293.3℃,为目标产物.更多还原

【Abstract】 Phthalic anhydride and urea were used as raw materials for the synthesis of 4-aminophthalimide via dehydration-cyclization,nitration by mixed acid and reduction by iron powder.In dehydration-cyclization reaction,catalyst and toluene as dehydrater were added,and water was steamed out by reflux,thus the reaction time was reduced.The yield was 98.0 %.Meanwhile,phosphoric anhydride was used as water absorbent in nitration,so the needed amount of concentrated sulfuric acid decreased in a half,the yield was more than 80.0 %.Finally,the ammonium chloride was added as electrolyte and pH value was adjusted to 4~5 by dropping concentrated chlorhydric acid in reduction,so iron powder was activated adequately,and the yield was 91.1 %.The target compound was characterized by differential scanning calorimetry(DSC) and Fourier transform infrared spectrometry(FT-IR).Experimental results indicat that the melting point of the product is 293.3 ℃.更多还原