摘要
3-噻吩丙二酸是β-内酰胺类抗生素替卡西林钠的重要侧链中间体,介绍了用简单、易行的合成路线进行3-噻吩丙二酸的合成研究。由3-溴噻吩制得3-碘代噻吩的过程中,通过实验发现最佳反应条件如下:噻吩、CuI的物质的量比为1∶1.5,原料浓度为1.5mol/L(溶剂为喹啉),反应时间为20h,反应温度为140℃时,反应收率可由原来的42.0%提高到68.3%。其熔点与文献报道一致,结构经红外光谱、核磁共振谱得以确认。中试较小试收率提高2.78%。
A simple and feasible synthesis process was selected for β-thienylmalonic acid, which is the key side-chain intermedi ate of semi-synthetic βlactam antibiotic-ticarcillin sodium. The best reaction conditions of preparing β-iodothiophene from β- bromothiophene are as follows： the mol ratio of β-bromothiophene to CuI is 1： 1.5, the concentration of the starting material is 1.5 mol/L in quinoline, the reaction time is 20 h and the temperature is 140 ℃. The yield can be raised up to 68.3% from 42.0 %. Its melting point is in line with the literature reported, and its structure is confirmed by infrared spectroscopy and nu clear magnetic resonance spectroscopy. The mid test yield is improved by 2, 78 % contrast to small rest experiment.
出处
《河北工业科技》
CAS
2012年第6期381-384,共4页
Hebei Journal of Industrial Science and Technology
