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NH4Cl作为电解质,滴加浓HCl,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.
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℃.
出处
《南京工业大学学报(自然科学版)》
CAS
2008年第6期51-53,共3页
Journal of Nanjing Tech University(Natural Science Edition)