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2-氯-3-氰基吡啶的合成
引用本文:刘振香,蔡春.2-氯-3-氰基吡啶的合成[J].精细化工中间体,2005,35(3):28-30.
作者姓名:刘振香  蔡春
作者单位:南京理工大学,化工学院,江苏,南京,210094;南京理工大学,化工学院,江苏,南京,210094
摘    要:烟酰胺与双氧水在冰醋酸中反应生成N-氧化烟酰胺(1),适宜的反应条件是烟酰胺∶双氧水=1∶1.5(mol/mol),冰醋酸的用量为50 ml(烟酰胺用量5.0 g),反应时间为4h,收率80.6%;化合物1再与五氯化磷和三氯氧磷反应合成了2-氯-3-氰基吡啶(2),适宜的反应条件为N-氧化烟酰胺∶五氯化磷∶三氯氧磷=1∶1.7∶5.0(mol/mol),反应时间为2.0h,收率48.9%。

关 键 词:烟酰胺  氧化  N-氧化烟酰胺  2-氯-3-氰基吡啶
文章编号:1009-9212(2005)02-0028-03
修稿时间:2004年12月4日

Synthesis of 2-chloronicotinonitrile
LIU Zhen-xiang,CAI Chun.Synthesis of 2-chloronicotinonitrile[J].Fine Chemical Intermediates,2005,35(3):28-30.
Authors:LIU Zhen-xiang  CAI Chun
Abstract:Nicotinamide-N-oxide (1) was prepared by oxidizing nicotinamide in the glacial acetic acid (AcOH) by 30% H_(2)O_(2).The reaction conditions recommended were as follow: the molar ratio of nicotinamide to H_(2)O_(2)was 1:1.5, amount of AcOH 50 ml (nicotinamide 5.0 g), reaction time 4 h, and the yield 80.6%. Treatment of the compound 1 with a mixture of phosphorus pentachloride and phosphorus oxychloride gave 2-chloronicotinonitrile (2), and the reaction conditions recommended were as follow: the molar ratio of Nicotinamide-N-oxide to phosphorus pentachloride, phosphorus oxychloride was 1∶1.7∶5.0, reaction time 2.0 h, and the yield reached 48.9%.
Keywords:Nicotinamide  oxidation  Nicotinamide-N-oxide  synthetize  2-chloronicotinonitrile
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