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Optically active α-amino acid was asymmetrically synthesized under soluble polymer-supported quinine by homogeneous phase catalytic reaction. The precursor of l -phenylalanine, Ph 2 NCH(CH 2 Ph)CO 2 C 2 H 5 (C 24 H 23 NO 2 , M r =364.38) has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic system with space group P 2 1 / c , a =10.4539(10), b =9.8315(10), c =19.8896(19) A, α =90.00, β =93.661(2), γ =90.00°, V =2040.0(3) A 3 , Z =4, D c =1.164 mg mm −3 , μ =0.074 mm −1 , F (000)=760. The final R and wR factors are 0.0463 and 0.1239, respectively, with 3610 ( R int =0.0291) independent reflections.