摘要
以过氧化氢为氧化剂,在稀碱条件下将2-氰基-3-甲基吡啶不完全水解形成3-甲基-2-吡啶甲酰胺,然后用新制备的次溴酸钠进行霍夫曼降解,获得标题化合物2-氨基-3-甲基吡啶。比较适宜的反应条件(反应温度,氢氧化钠浓度,反应时间)水解反应:50°C,5%,3.5 h,H2O2浓度为10%;霍夫曼降解反应:60°C,12%,0.5 h。摩尔总收率达74%,并通过GC-MSI、R、和1H NMR确证结构。
2-Amino-3-methyl pyridine was prepared with 2-cyano-methylpyridine as raw material via hydrolysis in dilute basic solution using H2O2 as oxidant and Hofmann degradation with NaBrO. The feasible reaction conditions were as follows ： hydrolysis, 50℃, 5% NaOH, 3.5h, 10 % of H2O2 ; Hofmann degradation, 60℃, 12 % NaOH, 0.5 h. The overall yield was 74% （mol）. The product obtained was identified by GC-MS,IR,^1H NMR and elemental analysis.
出处
《化学世界》
CAS
CSCD
北大核心
2006年第2期105-107,共3页
Chemical World
