Su Dai-guo
2012
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Journal
Hebei Journal of Industrial Science and Technology
Abstract
A simple and feasible synthesis process was selected for 3-thienylmalonic acid,which is the key side-chain intermediate of semi-synthetic β-lactam antibiotic-ticarcillin sodium.The best reaction conditions of preparing 3-iodothiophene from 3-bromothiophene are as follows: the mol ratio of 3-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 nuclear magnetic resonance spectroscopy.The mid test yield is improved by 2.78% contrast to small test experiment.