Empty fruit bunch (EFB), which is one of the primary agricultural wastes generated from the palm oil plantation, is generally discharged into the open environment or ends up in landfills. The utilization of this EFB waste for other value-added applications such as activated carbon and biofuels remain low, despite extensive research efforts. One of the reasons is that the EFB is highly vulnerable to microbial and fungi degradation under natural environment owning to its inherent characteristic of high organic matter and moisture content. This can rapidly deteriorate its quality and results in poor performance when processed into other products. However, the lignocellulosic components in degraded EFB (DEFB) still largely remain intact. Consequently, it could become a promising feedstock for production of bio-products after suitable pretreatment with organic solvents. In this study, DEFB was subjected to five different types of organic solvents for the pretreatment, including ethanol, ethylene glycol, 2-propanol, acetic acid and acetone. The effects of temperature and residence time were also investigated during the pretreatment. Organosolv pretreatment in ethylene glycol (50 v/v%) with the addition of NaOH (3 v/v%) as an alkaline catalyst successfully detached 81.5 wt.% hemicellulose and 75.1 wt.% lignin. As high as 90.4 wt.% cellulose was also successfully retrieved at mild temperature (80 °C) and short duration (45 min), while the purity of cellulose in treated DEFB was recorded at 84.3%. High-purity lignin was successfully recovered from the pretreatment liquor by using sulfuric acid for precipitation. The amount of recovered lignin from alkaline ethylene glycol liquor was 74.6% at pH 2.0. The high recovery of cellulose and lignin in DEFB by using organosolv pretreatment rendered it as one of the suitable feedstocks to be applied in downstream biorefinery processes. This can be further investigated in more detailed studies in the future.