This study introduces the catalyst-free production of levulinic acid (LA) and formic acid (FA) from spent coffee grounds (SCGs) as a starting material in a biphasic system of 1,2-dichloroethane (DCE)-water at temperatures above 160 degrees C. In addition to the advantage of using the biphasic system attributed to the product equilibrium, DCE served as a source of hydrogen induced by subcritical water (SCW). The effect of temperature, the amount of DIW and DCE, and the pretreatment on SCG (raw or lipid extracted SCG (LE-SCG)) on the overall reaction and humin formation were studied. The maximum conversion of LA and FA was 47 and 29 w/w% of the total convertible monosaccharides in raw SCGs while 43 and 28 w/w% of the conversion were obtained at 180 degrees C when LE-SCG was used. The solvothermal effects of two media provides a non-catalytic route to utilize undried SCG for the production of LA and FA.