摘要
以氨基脲盐酸盐-(2-13C,15 N3)为原料,经与苯甲醛缩合,在乙醇钠催化作用下,与氯乙酸乙酯缩合环化制得1-苯亚甲基氨基乙内酰脲,最后盐酸水解,制得1-氨基乙内酰脲盐酸盐-(2-13 C,15 N3)。合成路线优势在于反应条件温和,产物总收率高于65%。产品经IR、HPLC、NMR和MS表征结果表明:化学纯度>98.4%,13C同位素丰度>98%,15 N同位素丰度>99%。
A novel and mild synthesis method of AHD·HCl-（2-13C,15N3） was described.The intermediate was prepared by condensation of semicarbazide-（13C,15N3） with phenylaldehyde.Then,1-benzylideneaminohydantion was prepared by cyclization condensation with ethyl monochloroacetate in presence of sodium ethoxide.At last,AHD·HCl-（2-13C,15N3） was prepared by hydrolysis with hydrochloric acid.The yield of AHD·HCl-（2-13C,15N3） was more than 65%.The product was characterized by IR,HPLC,NMR and MS,and its purity was more than 98.4%.The 13C and 15N enrichment was more than 98% and 99%,respectively.
出处
《化学世界》
CAS
CSCD
北大核心
2012年第10期624-628,共5页
Chemical World
基金
国家科技支撑计划课题项目(2009BAK61B04)
作者简介
徐建飞（1979-），男，上海人，硕士生，化学工程专业。E-mail：xujianfei100@163．com；
E-mail：xiaoningdu@163．com
