摘要
该文"一锅煮"合成13C标记甘氨胆酸。即以氯甲酸异丁酯为活化试剂,甘氨酸-1-13C和胆酸直接缩合制备甘氨胆酸-甘氨酰基-1-13C,合成产品使用HPLC、LC-MS和1HNMR等进行分析。优化的合成条件为:n(氯甲酸异丁酯)∶n(胆酸)∶n(甘氨酸)∶n(三乙胺)=1∶1∶1∶1,反应温度10℃,反应时间1 h,13C标记甘氨胆酸收率82.4%(以甘氨酸-1-13C计),13C丰度达99.1%atom13C,光学纯度99.2%,w(甘氨胆酸-甘氨酰基-1-13C)=97.7%。
With isobutyl chloroformate as the active agent,glycocholic acid-glycyl-1-13C,a 13C-breath test substrate and applications in clinical practice,was synthesized by ＂one pot＂ method of the condensation of glycine-1-13C directly with cholic acid.13C labelled glycocholic acid was characterized by HPLC,LC-MS and 1HNMR.The yield of 13C labelled glycocholic acid was 82.4%（based on glycine-1-13C）,with 99.1% atom 13C abundance,99.2% optical purity and 97.7% chemical purity,at the optimized conditions,which were n（isobutyl chloroformate）∶n（cholic acid）∶n（glycine）∶n（triethylamine）=1∶1∶1∶1,10 ℃ reaction temperature and 1 h reaction time.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2010年第12期1216-1219,共4页
Fine Chemicals
基金
国家高技术研究发展计划项目(2008AA02Z427)~~
