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6-苯基-5-氯-3(2H)-哒嗪酮合成工艺的改进
引用本文:李树白,贺新,薛叙明,王斐斐,聂华丽.6-苯基-5-氯-3(2H)-哒嗪酮合成工艺的改进[J].化学试剂,2011,33(4):353-355.
作者姓名:李树白  贺新  薛叙明  王斐斐  聂华丽
作者单位:1. 常州工程职业技术学院,化工系,江苏,常州,213164
2. 东华大学化学化工与生物工程学院,上海,201620;东华大学生态纺织教育部重点实验室,上海,201620
基金项目:国家自然科学基金资助项目(50773009); 上海市科委基金资助项目(08JC1400600); 中央高校专项基金和教育部博士点新教师基金资助项目(2009007512001); 常州工程职业技术学院2010年度第一批次院级科研课题资助项目(KJY-19)
摘    要:6-苯基-3-哒嗪酮经三氯化磷和氯气氯代,所得中间体6-苯基-3,5-二氯哒嗪经氢氧化钠皂化、盐酸酸化制得标题化合物,通过回收皂化反应的副产物6-苯基-3-氯-5-羟基哒嗪作为氯代反应的原料,总收率56.6%,考察了回收物料及氯气流量对氯代反应的影响,讨论了皂化产物的分离工艺,最终产物经1HNMR结构确证.

关 键 词:6-苯基-5-氯-3(2H)-哒嗪酮  6-苯基-3-哒嗪酮  合成

Improvement of synthesis process for 6-phenyl-5-chloro-3-pyridazone
LI Shu-bai,HE Xin,XUE Xu-ming,WANG Fei-fei,NIE hua-li.Improvement of synthesis process for 6-phenyl-5-chloro-3-pyridazone[J].Chemical Reagents,2011,33(4):353-355.
Authors:LI Shu-bai  HE Xin  XUE Xu-ming  WANG Fei-fei  NIE hua-li
Affiliation:LI Shu-bai*1,HE Xin1,XUE Xu-ming1,WANG Fei-fei1,NIE hua-li2a,2b(1.Department of Chemical Engineering,Changzhou Institute of Engineering Technology,Changzhou 213164,China,2.Donghua University,a.College of Chemistry,Chemical Engineering and Biotechnology,b.Key Laboratory of Science & Technology of Eco-Textile(Donghua University),Ministry of Education,Shanghai 201620,China)
Abstract:6-Phenyl-5-chloro-3(2H)-pyridazone was synthesized from 6-phenyl-3-pyridazone by chlorination with chlorine and phosphorus trichloride to give 3-phenyl-4,6-dichloropyridazine which saponified with sodium hydroxide,followed by acidified with HCl,the overall yield is 56.6% by recycling isomer 6-phenyl-3-chloro-5-hydroxylpyridazine from saponifination as raw material used in chlorination.Effects of recycled by-product and flow rate of chlorine in chlorination on yield were investigated,separation procedure of ...
Keywords:6-phenyl-5-chloro-3(2H)-pyridazone  6-phenyl-3-pyridazone  synthesis  
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