Biomass synthesis of palm empty fruit bunch (PEFB) into sugars yield as raw material for bioethanol conversion has successfully been performed through organosolv pretreatment and acid hydrolysis processes. These synthesis processes were conducted to evaluate the effect of solvent concentration namely ethanol (C2H5OH) and sulfuric acid (H2SO4), reactions time and temperature against total sugars yield. It is optimized through pretreatment and hydrolysis processes, respectively. The optimum total sugars for pretreatment optimization was obtained 98.89 mg/L which correspond to 55% vol of C2H5OH with reaction time of 60 min at 120 degrees C. Hydrolysis process for pretreatment optimization was conducted at 1% vol H2SO4, reaction time of 30 min and temperature of 90 degrees C. The optimum pretreatment conditions were selected for further hydrolysis process with H2SO4 to optimize sugars yield amount in the slurries. The results of acid hydrolysis showed that the optimum amount of total sugars obtained was 133.17 mg/L at concentration H2SO4 0.5% vol with reaction time 30 min and temperature 100 degrees C. Therefore, it is concluded that organosolv pretreatment and acid hydrolysis can be used as a novel integrated method to optimize the total sugars production synthesized from PEFB to bioethanol. (C) 2016 Published by Elsevier Ltd.