摘要
4-硝基邻苯二甲酰亚胺是一精细化工中间体,继续反应可得到5-氨基邻苯二甲酰亚胺和5-氰基苯酞等重要的精细化工产品,前者可用于制备偶氮系列的染料,后者可用于制备药物Citalopram。通过用混酸对邻苯二甲酰亚胺进行硝化,制备了4-硝基邻苯二甲酰亚胺。对反应时间、反应温度和混酸配比等工艺参数对硝化反应的影响进行了考察,并优化了工艺条件。在反应温度为25℃,反应时间为10h,混酸中硝酸∶硫酸=1∶4.5时,产物的收率达到82%以上,比文献报道的60%的收率有了较大的提高。产物的熔点为192.1～192.7℃,其红外谱图与标准谱图相一致。
The title compound is an intermediate of fine chemicals by which \{5\|aminophthalimide\} and 5\|cyanophthalide can be made. The former may be used to prepare azo\|dye and the latter in the synthesis of Citalopram. 4\|Nitrophthalimide was prepared through nitration of o\|phthalimide by mixed acid. The influences of reaction time, temperatures and the proportion of mixed acid were studied; and the operation conditions were optimized. The yield was raised to more than 82 % compared with the 60 % in the literature. The optimum conditions were as follows: with a mixed acid of nitric acid∶sulfuric acid=1∶45 in the course of 25 ℃ and 10 h. The melting point of the product was 192.1～192.7 ℃, and the IR was identical with the standard spectrum.
出处
《浙江工业大学学报》
CAS
2003年第5期512-514,523,共4页
Journal of Zhejiang University of Technology
