| N-(6-氯-1-氧-3-吡啶甲基)邻苯二甲酰亚胺的合成 |
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| 引用本文： | 吕兆萍,李国华,杨红.N-(6-氯-1-氧-3-吡啶甲基)邻苯二甲酰亚胺的合成[J].精细化工,2006,23(3):307-309,312. |
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| 作者姓名： | 吕兆萍 李国华 杨红 |
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| 作者单位： | 1. 南京农业大学,理学院,江苏,南京,210095;南京航空航天大学,材料科学与技术学院,应用化学系,江苏,南京,210016
2. 南京农业大学,理学院,江苏,南京,210095 |
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| 摘 要： | 以邻苯二甲酰亚胺为起始原料,在常温条件下与氢氧化钾反应合成了邻苯二甲酰亚胺钾,其熔点352.8~353.4℃,收率95%。然后在70℃和微波辐射条件下,以邻苯二甲酰亚胺钾作为亲核试剂,与2-氯-5-氯甲基吡啶反应20 m in,制备了N-(6-氯-3-吡啶甲基)邻苯二甲酰亚胺,熔点140.3~140.5℃,收率98.5%。最后以双氧水为氧化剂,在75℃条件下,N原子氧化,合成了目标产物N-(6-氯-1-氧-3-吡啶甲基)邻苯二甲酰亚胺,熔点138.2~139.4℃,收率92%。利用红外光谱(FTIR)、核磁共振氢谱(1HNMR)、气-质联用仪(GC-MS)解析并确定了中间产物及目标化合物的结构。
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| 关 键 词： | N-(6-氯-1-氧-3-吡啶甲基)邻苯二甲酰亚胺 亲核取代反应 微波辐射 氧化反应 |
| 文章编号： | 1003-5214（2006）03-0307-04 |
| 收稿时间： | 2005-08-09 |
| 修稿时间： | 2005-08-092005-09-23 |
Synthesis of N-(6-Chloro-1-oxy-3-pyridinemethyl) phthalimide |
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| L Zhao-ping,LI Guo- hua,YANG Hong.Synthesis of N-(6-Chloro-1-oxy-3-pyridinemethyl) phthalimide[J].Fine Chemicals,2006,23(3):307-309,312. |
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| Authors: | L Zhao-ping LI Guo- hua YANG Hong |
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| Affiliation: | 1. College of Science, Nanjing Agricultural University, Nanjing 210095, Jiangsu, China; 2. College of Material Science and Engineering, Nanjing University of Aeronautics and Astronautics, Nanjing 210016, Jiangsu , China |
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| Abstract: | Potassium phthalimide(Ⅰ) was prepared at first from phthalimide by reacting with KOH in 95% yield,melting point 352.8～353.4 ℃.Then,nucleophilic substitution of 2-chloro-5-methylpyridine with Ⅰ at 70 ℃ under microwave irradiation gave N-(6-chloro-3-pyridinemethyl)phthalimide(Ⅱ) in 98% yield,melting point 140.3～140.5 ℃.Finally,oxidation of Ⅱ on nitrogen atom with H_2O_2 at 75 ℃ gave the target product N-(6-chloro-1-oxy3-pyridinemethyl)phthalimide in 98% yield,melting point 138.2～139.4 ℃.Structures of the intermediates and target product were characterized by FTIR,~1HNMR and GC-MS. |
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| Keywords: | N-(6-chloro-1-oxy-3-pyridinemethyl)phthalimide nucleophilic substitution microwave irradiation oxidation reaction |
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