^(13)C-甲醇的制备  

Synthesis of ^(13)C-labeled Methanol

作　　者：罗勇[1] 杜晓宁[1] 宋家龙[1] 陆平晔[1] 李美华[1] 

机构地区：[1]上海化工研究院,上海200062

出　　处：《同位素》2012年第4期214-218,共5页Journal of Isotopes

基　　金："十一五"国家科技支撑计划(2009BAK61B04);科技部转制院所专项(2011EG116066)

摘　　要：采用自制的催化剂和自行设计的高效催化反应器,用催化加氢的方法,以Ba13 CO3为原料制备了13 C-甲醇。所得甲醇水溶液在微型高效精馏反应器中进一步提纯后,得到的13 C-甲醇化学纯度>99.5%。实验设计的合成路线反应条件温和,同位素利用率>90%。13 C-甲醇经色质联用(GC-MS)和核磁(1 H NMR)检测,13 C同位素丰度>97%,13 C-甲醇的同位素丰度与原料相比降低<1%。以上结果表明,采用自制的催化剂和自行设计的高效催化反应器,成功地用催化加氢的方法,制备得到了13 C-甲醇。A novel convenient method for the synthesis of ^-methanol was described.^13C-methanol was prepared by means of catalytic hydrogenation,and then as-synthesized methanol solution was further purified in a microscale high-efficient rectification column.The chemical purity of ^13C-methanol was more than 99.5%.The synthetic route was featured by mild conditions and high yields of more than 90% based on isotopic substrate consumed.The product was characterized by GC-MS and 1H NMR,and the ^13C abundance of ^13C-methanol was more than 97%.Compared with the raw materials,the reduction of relative isotopic abundance of product was less than 1%.

关 键 词：13C标记 甲醇 催化加氢 

分 类 号：O628.2[理学—有机化学]