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作 者:张文雯[1] 叶爱英[1] 陈绘如[1] ZHANG Wen-wen , YE Ai-ying, CHEN Hui-ru(Institute of Pharmaceutical and Environmental Engineering,Changzhou Vocational Institute of Engineering, Changzhou 213164, Chin)
出 处:《化学试剂》2018年第5期491-494,共4页Chemical Reagents
基 金:常州市第十七批科技计划(科技支撑-社会发展)项目(CE20135011);常州工程职业技术学院科技项目(11130300317001);常州工程职业技术学院“化学原料药小试技术教学团队”、“绿色化学及应用酶科技创新团队”项目(11130800217001)
摘 要:以L-半胱氨酸为原料合成L-噻唑烷-4-甲酸后,与L-焦谷氨酸在负载型阳离子交换树脂催化下合成匹多莫德。研究了以负载Zn Cl2的凝胶型低交联度大交换量的阳离子交换树脂为催化剂合成匹多莫德的工艺条件。结果表明,当n(L-焦谷氨酸)∶n(L-噻唑烷-4-甲酸)=1.16∶1,以DMF为溶剂,催化剂用量为总物料的15.9%,在70℃反应2 h,匹多莫德总收率达69%,催化剂可重复使用。Started from L-cysteine to afford(R)-thiazolidine-4-carboxylic acid,which reacted with L-pyroglutamic acid to obtain pidotimod catalyzed by loaded cation exchange resin. The reaction conditions were investigated with ZnCl_2-loaded geltype,low crosslinking degree and high exchange capacity cation exchange resin as catalyst.Results reveal that the optimum reaction conditions was as follows: molar ration of L-pyroglutamic acid to(L)-thiazolidine-4-carboxylic acid 1. 16 ∶ 1,DMF as solvent,catalyst amount 15. 9% of total material,reaction temperature 70 ℃,reaction time 2 h. The total yield reached 69% and catalyst can be reused.
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