Efficient production of furfural from cornstalk in 2-Methyltetrahydrofuran/aqueous (MTHF/H 2O) biphasic system via parameter regulation (e.g., V MTHF/V H2O, temperature, time, and H 2SO 4 concentration) was proposed. The resulting solid residues achieved from the different MTHF/H 2O system conditions for furfural production were also to prepare glucose by adding cellulases to increase the high-value applications of cornstalk. A maximum furfural yield (68.1%) was obtained based on reaction condition (V MTHF:V H2O = 1:1, 170 °C, 60 min, 0.05 M H 2SO 4). Among these parameters, the concentration of H 2SO 4 had the most obvious effect on the furfural production. The glucose yields of the residues acquired from different MTHF/H 2O processes were enhanced and then a maximum value of 78.9% based on the maximum furfural production conditions was observed. Single factor may not be sufficient to detail the difference in glucose production, and several factors affected the hydrolysis efficiency of the residues. Overall, the MTHF/H 2O system effectively converted cornstalk into furfural and glucose via a simple and environment-friendly process, thus was an ideal manner for the food industries.