氘代氨基甲酸酯类化合物的合成与表征  

Synthesis and Characterization of Deuterated Carbamate Compounds

作　　者：徐建飞[1] 杜晓宁[1] 卢伟京[1] 王伟[1] 雷雯[1] 

机构地区：[1]上海化工研究院同位素研究所,上海200062

出　　处：《精细化工》2015年第8期954-956,960,共4页Fine Chemicals

基　　金：科技部科技支撑计划项目(2015BAK45B01);上海市科委地方攻关计划课题(14DZ0511800)~~

摘　　要：设计了以有机酚为原料制备氘代氨基甲酸酯类化合物的合成路线。有机酚（Ⅰa~Ⅰc）在Na OH催化作用下,经与三光气（BTC）反应,合成了中间体氯甲酸酯（Ⅱa~Ⅱc）,再与一甲胺-D3-盐酸盐缩合反应,制得目标化合物（Ⅲa＇~Ⅲc＇）。设计的合成路线避免使用异氰酸酯,且操作简单,工艺流程短,副产物少,收率可达60%以上,氘同位素丰度没有降低。产物经HPLC、MS、1HNMR和13CNMR表征,结果表明,化学纯度〉99%,氘同位素丰度〉99 atom%。A novel and mild synthesis method of deuterated carbamate compounds was oeslgneu, with organic phenol（ I a - I c） as raw materials, the intermediate chloroformate （ Ⅱ a - Ⅱ c） was prepared by the reaction of the raw materials with triphosgene under the catalysis of NaOH, and then the target carbamate compounds （ Ⅲa＇ ~ Ⅲ c＇） were obtained by condensation of the intermediate with methylamine_D3-hydrochloride. This synthesis route can avoid the use of highly toxic isocyanate, and has the advantages of simple operation, short process flow, less side product, the yield of carbamate compounds was more than 60%, and deuterium labeled isotope abundance being not diluted. The product was characterized by means of HPLC, MS,1HNMR and 13CNMR, which shows that the chemical purity was more than 99%, and the deuterium enrichment was more than 99 atom%.

关 键 词：氘代 异丙威 速灭威 仲丁威 精细化工中间体 

分 类 号：O621.3[理学—有机化学] R817[理学—化学]