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%。
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%.
出处
《精细化工中间体》
CAS
2005年第3期28-30,共3页
Fine Chemical Intermediates
