Study On Synthesis Of Phenylglycine By Landini Method

Phenylglycine and its derivates are important medicinal intermediate products, which can be used to synthesize some pesticides, poly-peptide hormone,β-lactam antibiotics such as ampicillin, cephallexin, cephradine. With the development of the antibiotic industry, the demand amount of Phenylglycine will increase steadily. So to research and develop the technology of Phenylglycine to be friendly to environment has a broad market perspective.Nowadays the methods to produce phenylglycine primarily include Phenylacetic Acid method, Glyoxylic Acid method, Asymmetry Synthesis method, Stereoselective Synthesis method, Enzyme method and Chloroform method. In this project Landini method is used to synthesize phenylglycine. This paper consists of two parts.Part 1: to establish the analytic method. First phenylglycine is identified by IR and GC-MS and then analyze the compositions of phenylglycine sample quantitatively. On the basis of comparing the accuracy of different analytical methods, such as fusing point determination method, titration method and HPLC method. HPLC method is selected to analyze the contents of phenylglycine in the experiment. The optimal analytic conditions are selected by investigating the effects of wave length, the ingredient of mobile phase and flow rate on detection and isolation.Part 2: to study the technology of synthesize phenylglycine. One step synthesis of phenylglycine from benzaldehyde, chloroform, sodium hydroxide and ammonia water in the presence of phase-transfer catalyst has been studied. First, three kinds of phase transfer catalysts, TBAB, BTEAC and CTMAB, are compared and screened according to the catalytic performance. TBAB is the best because of its best catalytic performance. The main factors of effecting phenylglycine yield are studied by orthogonal experiment. The results of visual and variance analysis show that the amount of sodium hydroxide and chloroform are main influence factors. In order to find the distribution of intermediates and its changing rule during reaction, the analysis of consecutive sampling is used to trace the whole reaction process. The optimal technological conditions are obtained by comparing the effects of various technological conditions, the amount of sodium hydroxide, chloroform, catalyst, the reaction time in ice bath, the reaction time in water bath, on the yield of phenylglycine with orthogonal experiment.