L-噻唑烷-4-甲酸乙酯盐酸盐的合成工艺研究

Research on the synthetic process of L-thiazolidine-4-formic acid ethyl ester hydrochloride

L-噻唑烷-4-甲酸乙酯盐酸盐是一种重要的含N、S杂环化合物,特殊的化学结构使其在绿色农药、免疫药物和新型材料等领域均具有广泛的应用前景。以L-半胱氨酸盐酸盐为原料,通过缩合反应和酯化反应两步合成L-噻唑烷-4-甲酸乙酯盐酸盐,通过单因素实验对L-噻唑烷-4-甲酸乙酯盐酸盐的合成工艺进行优化,通过熔点、红外光谱与质谱对产物进行表征,结果表明,缩合反应最佳合成条件:L-半胱氨酸盐酸盐∶甲醛为1∶1.2,反应温度为400℃,反应时间为4 h;酯化反应最佳合成条件:反应温度为700℃,反应时间为4 h;对两步反应产物进行表征与分析,判定分别是各步目标产物。该合成工艺对设备要求低,易操作,符合工业化大规模生产需要。

L-thiazolidine-4-formic acid ethyl ester hydrochloride is an important heterocyclic compound including N and S,widespreadly used in the fields of green pesticides,immune-medicine and new materials because of its special chemical structure.Through two reaction steps of condensation and esterification,L-thiazolidine-4-formic acid ethyl ester hydrochloride was synthetized with L-cysteine hydrochloride as the raw materials.By the method of single factor experiment,the synthesis process of L-margaret-4-formic acid ethyl ester hydrochloride was optimized,the products were characterized by melting point,IR spectrum and mass spectrum.The results show that the optimum synthetise conditions of condensation reaction are that the molar ratio of L-cysteine hydrochloride to formaldehyde,the reaction temperature and the reaction time are 1∶1.2,400℃and 4 h respectively.The optimum synthetise conditions of esterification reaction are that the reaction temperature and the reaction time are 700℃and 4 h respectively.The characterization results of the two step reaction products show that the products are respectively the target products.The equipments of the synthesis process are simple,and easy to operate.The process conforms to the industrialized mass production needs.