摘要
以15NH4Cl为同位素标记前体,经与苯甲酰氯胺化、霍夫曼降解得到15N标记苯胺,15N标记苯胺再与对甲苯磺酸酯进行甲基化反应,合成得到一种重要的同位素标记基础试剂15N-N,N-二甲基苯胺.以消耗的15NH4Cl计,三步反应总收率大于58.3%.产品结构经红外(IR)、核磁(NMR)、高效液相(HPLC)、质谱(MS)等表征进行确定,其化学纯度大于99.0%,同位素丰度大于98.4%15N.
An efficient synthesis of 15N-N,N-dimethylaniline with 15NH4Cl as the common substrate is reported.Ammoni-ation of benzoyl chloride with 15NH4Cl provided 15N-benzamide,which was converted to 15N-aniline by Hofmann degrada-tion.Methylation of 15N-aniline with methyl p-toluenesulfonate provided 15N-N,N-dimethylaniline.The overall yield of NMR,HPLC and MS to be target compound.Its chemical purity is higher than 99.0% and isotopic enrichment is higher than 98.4% 15N.
出处
《有机化学》
SCIE
CAS
CSCD
北大核心
2012年第1期145-148,共4页
Chinese Journal of Organic Chemistry
基金
科技部转制院所专项(No.2011EG116066)
质检总局科技专项(No.2009IK134)资助项目~~
关键词
同位素标记
合成
N
N-二甲基苯胺
表征
甲基化
isotope-labeled
synthesis
N
N-dimethylaniline
characterization
methylation
