摘要
实验以2-氨基吡啶为原料,经N-酰化、溴代及酰基水解一锅法合成了2-氨基-5-溴吡啶。N-酰化在回流条件下进行,n(醋酐):n(2-氨基吡啶)=1.6:1;溴代温度为50℃,n(液溴):n(2-氨基吡啶)=1.1:1;水解在室温下进行,氢氧化钠浓度为40%,总收率66.5%。产物结构经红外光谱及核磁共振氢谱进行了确证。
2-Amino-5-bromopyridine and its derivatives are important pharmacentical and chemical in- termediates, which are prepared with 2-aminopyridine as raw materials by N-acylation, bromination and hydrolization. N-acylation was carried out under reflux condition, n(aceticanhydride) : n(2- aminopyridine)=1. 6 : 1; bromination at 50 ℃, n(Br2) : n(2-aminopyridine)=1.1 : 1; hydrolization at room temperature, the concentration of NaOH was 50%. The total yield was 66.5%. The structure of product was identified by IR and ^1H NMR.
出处
《精细石油化工》
CAS
CSCD
北大核心
2010年第4期4-6,共3页
Speciality Petrochemicals