Abstract: According to some research achievements, a green oximation comprehensive experiment was designed to overcome the shortcomings of the traditional oximation reaction, and the base and reaction equipment were improved. Recyclable nano-K₂CO₃ was prepared firstly by ultrafine wet milling and characterized by the laser particle size analyzer, scanning electronic microscopy (SEM), and CO₂-TPD. The synthesis of ethyl α-(hydroxyimino)benzenepropanoate was performed using nano-K₂CO₃ as the base. The preparation of ethyl nitrite and oximation of diethyl benzylmalonate were carried out simultaneously by series devices. The experiment avoids the shortcomings of sodium alkoxides that cannot be recovered and corrodes equipment, and solves the problems of storage and transportation difficulties and easy environmental pollution of volatile nitrite. This comprehensive experiment is beneficial for students to learn the idea of environment-friendly green chemistry, improve the students’ comprehensive ability and quality, and cultivate their scientific research innovation thinking ability.