摘要
合成碘代酪氨酸的甲基替代体,研究其合理的合成路线,确定最佳反应条件对甲状腺激素类药物的生产有很大的意义.合成了甲状腺激素类药物的中间体3,5-二甲基-DL-酪氨酸(DL-Dmtyr),确定了其适宜的合成条件是:通入HCl 20h,4-氯甲基-2,6-二甲基-茴香醚可获得较高的产率;加热回流6 h,且在冰水中静置的时间足够长,α-乙酰氨-α-(4-甲氧基-3,5-二甲基苄基)丙二酸乙酯产率较高,从热的正己烷中反复重结晶可获得纯度较高的纯品;氢碘酸用量应为理论用量的1.5倍,裂解反应时间为16h.
It is very important for the contrastive research of weak interaction between ligands to synthesize the methyl tyrosine to replace iodine tyrosine in complexes. In this thesis, 3,5 - dimethyl - DL- tyrosine（DL- Dmtyr） is synthesized through three step route, and purifi certain：if hydrogen chloride gas is passed through ed by for 20 recrystallization. Also, the best reaction condition is made h, 3,5 - dimethyl - 4 - methoxybenzyl chloride can be obtain most; if the preceding ester is heated under reflux for 6 h, then deposit the mixture enough in ice water, the maximum of α - acetamido - α - （3,5 - dimethyl -4 - methoxybenzyl）malonate can be obtained;the dosage of hydriodic acid should be one and a half of theory,reaction mixture should be heated under reflux 16 h.
出处
《辽宁大学学报（自然科学版）》
CAS
2007年第1期74-77,共4页
Journal of Liaoning University：Natural Sciences Edition
基金
国家自然科学基金资助(No:29971014)
