稳定同位素标记^(13)C_6-结晶紫和^(13)C_6-隐色结晶紫的合成  

Syntheses of Labeled ^(13)C_6-Crystal Violet and ^(13)C_6-Leucocrystal Violet

作　　者：罗勇[1] 杨维成[1] 刘卫霞[1] 

机构地区：[1]上海化工研究院技术开发中心,上海200062

出　　处：《精细化工》2011年第10期950-953,990,共5页Fine Chemicals

基　　金：科技部转制院所专项(2009EG116086);上海市科委科技创新行动计划(09dz2200700)~~

摘　　要：以13C-甲醇为前体,通过磺酸酯活化方法得到13C2-N,N-二甲基苯胺,再进一步缩合得到13C6-隐色结晶紫,继续氧化后得13C6-结晶紫。以消耗的13CH3OH计算,13C6-隐色结晶紫和13C6-结晶紫的总收率分别为39.9%和21.9%。产品结构经质谱和核磁共振波谱等表征确定,色谱纯度高于99.0%,同位素丰度高于98.5%,可作为食品安全领域检测用同位素内标试剂。This article presents efficient syntheses of two labeled standards, ^13C6-leucocrystal violet and ^13C6-violet crystal,with 13CH3OH as the common substrate. Esterification of p-toluenesulfonyl chloride with ^13CH3OH provided ^13C-methyl p-toluenesulfonate, which was subsequently used to methylate aniline to give ^13C2-N, N-dimethylaniline. Condensation of ^13C2-N, N-dimethylaniline afforded ^13C6- leucocrystal violet, which was further converted into ^13 C6-violet crystal by oxidation. The yields of ^13 C6- leueocrystal violet and ^13C6-violet crystal were 39.9% and 21.9% respectively based on ^13CH3OH consumed. Both products were confirmed by NMR and LC-MS to be target compounds. Their chemical purity is higher than 99.0 % and isotopic enrichment is higher than 98.5 %. The above compounds could be used as internal standards in the field of food safety testing.

关 键 词：同位素标记 结晶紫 隐色结晶紫 表征 功能材料 

分 类 号：TQ421.6[化学工程] O628.2[理学—有机化学]