A Disquisition For Synthesis Of Cinnamic Acid From Styrene And Carbon Tetrachloride

According to previous research, Cinnamic Acid ,was synthesized by using styrene and carbon tetrachloride as raw material. The Cinnamic Acid was synthesized by using cuprum chloridize, diethylamine andγoxide-alumina, pyridine, iso-propanol as catalyst through addition and alcoholysis reaction in research. That have been throughly studied influence of reaction temperature, time, reactant ratio, catalyst quantity and the catalyst type...etc.. Using orthogonal experiment identified the optimized reaction condition and gave a preliminary analysis on the mechanism of reaction. When using cuprum chloridize and diethylamine as catalyst, the optimum reaction condition is that reaction temperature 70~75℃, time 4 h, reactant mole ratio 1:2.5, catalyst quantity 2% and the yield is 88.51%; When usingγoxide-alumina, pyridine, iso-propanol as catalyst, the optimum reaction condition is that reaction temperature 70~75℃, time 5 h, solvent ratio 1:2, catalyst quantity 4%, and the yield is 93.06%. The process which the production was synthesized by usingγalumina, pyridine, iso-propanol as catalyst was commend. In second alcoholysis reaction, The final production was synthesized by using methyl sulfonicbenzene-vitriol and reaction time is15 h, the yield is 92.34%; Using vitriol- vinegar, reaction time is 13 h, which give the yield of 72.86%, but can get intact crystallogeny;Using iron vitriol- vinegar, reaction time is short, which give the yield of 91.35%, but could not get pure colour; Using zinc sulfate–vinegar, reaction time is short, which give the yield of 91.74%. If two processes are according with the optimized process technical conditin, final rate give the yield of 86%.In the course of reaction, intermediate and manufacture were separated and purified by the second crystal. The final production was identified by the information provided from FTIR , gas chromatography, liquid phase chromatography and mensurating melting point . The results shows that the final production are intermediate.At last, by pure the l,3,3,3–tetrachloropropyl benzene and Cinnamic Acid, structure of reagent and reference, extrapolate infer reaction mechanism and validate it by experimentation result. It shows the synthesize ways are reasonable.