Abstract As the optical enantiomers in the biological activity, toxicity and mechanism of the metabolism is different, so a single enantiomer preparation of paramount importance. The chiral α-phenylethylamine is a complex preparation of single enantiomers, one of the important intermediate, which can be raceme chiral separation of the reagents, but also for the asymmetric synthesis of chiral materials, it Preparation and analysis of great significance. In this paper, the use of tartaric acid and cinnamic acid, respectively, were split on their research. In this paper, first of all from racemic α-phenylethylamine start the preparation, through the reaction of Mr Carter, the use of ammonium perchlorate and a mixture of acetophenone check the heating system of α-phenylethylamine. Experiment temperature control is key to the success of the experiment, the reaction temperature must be controlled at 180 ℃ -185 ℃. After repeated failures in this experiment, the ultimate success of the preparation of the α-phenylethylamine, the yield was 41.9%. In the separation experiment, I chose the commonly used laboratory method of chemical separation, separation agent of choice for the tartaric acid and cinnamic acid, and the two agents split the effect of separation were compared, except for some man-made factors can be identified in the laboratory using a small amount of cinnamic acid to the preparation of optically active α-phenylethylamine in the operation of the experimental and synthetic results, the split method is better than some of tartaric acid. Tartaric acid obtained by resolution of the experiment the S-(-) - - Optical Rotation for phenylethylamine α25D = 1.2, the density of d = 0.0676g/ml, [α] D25 = 17.75, Polarimetry purity 44.22%, cinnamic acid removed sub-experiments, R-α-phenylethylamine and S-α-phenylethylamine, respectively, for the optically active purity 78.1% and 81.5% Also in the experiment, I modified the experimental book unreasonable on this experiment, such as acetophenone and in the Ammonium reaction after washing use a mixture of organic matter back to the lower reaction bottle, and the water layer is extraction with chloroform 2 times, and then extract the response back to distillation bottles, but in practice it is difficult to carry out distillation, low boiling point because of chloroform (61.7 ℃). If the temperature controlled easy to dry reactant, in the operation more difficult. Also compare the toxicity of chloroform, and, therefore, I chose a relatively high boiling point and relatively low toxicity of toluene as the extractant (110.8 ℃). In the experiment to reduce the difficulty of the operation. Key word: α-Benzene ethylamine Chiral synthesis Chiral resolution