摘要
以L-组氨酸(L-His)为原料,水杨醛作催化剂,在乙酸溶剂中,与(R)-酒石酸((R)-TA)反应制得D-His.(R)-TA。讨论了反应温度、反应时间、不同的溶剂和催化剂的用量对反应结果的影响,确定了制备D-His.(R)-TA的最佳工艺条件为L-His:(R)-TA:水杨醛=1∶1∶0.1(mol),反应温度为90℃,反应时间为3 h。中间体盐D-His.(R)-TA在甲醇中用三乙胺处理得D-组氨酸,总收率为94.2%,光学纯度为98.7%。
D-His. ( R )-TA salt was obtained by reaction of L-His with ( R )-TA in acetic acid in the presence of salicylaldehyde as catalyst. The influences of time, temperature, solvents and catalyst dosage on the reaction were investigated. The optimum reaction conditions are as follows: L-His: (R)-TA: salicylaldehyde = 1 : 1:0.1 (mol); reaction temperature, 90℃ ; and reaction time, 3 h. Treatmet of the obtained D-His- ( R)-TA salt with methanol solution of triethylamine gave D-His with 98.7% optical purity and 94.2% yield based on the starting L-His.
出处
《化学世界》
CAS
CSCD
北大核心
2006年第6期352-354,360,共4页
Chemical World
关键词
D-组氨酸
不对称转化
消旋
水杨醛
D-histidine
asymmetric transformation
racemization
salicylaldehyde