Chloride vapor phase epitaxy of Ga0.52In0.48P/GaAs was studied using a reactor with two growth chambers. We have obtained high‐purity epitaxial layers of both GaInP and GaAs. For the growth of a heterostructure with an abrupt interface, the optimum growth condition was investigated in detail. Abruptness of the heterointerface was investigated by observing the two‐dimensional electron gas at the heterointerface of Ga0.52In0.48P/GaAs by the Hall and Shubnikov–de Haas measurements.