We investigated the extraction of para-coumaric acid (pCA) from different agriculture residues (corn stover, sugarcane bagasse, sorghum stalk, pearl millet stalk, green gram shell, groundnut shell, sesame shell) using sugarcane bagasse alkaline hydrolysis and separation of pCA using sugaring out - a new phase separation method. Primary screening of different feed stocks was by alkaline hydrolysis with 2M NaOH for 6 h at room temperature. Sugarcane baggase resulted into significant amount of pCA (1.1 g/L) and small amount of ferulic acid (FA) (0.23 g/L). The optimized alkaline hydrolysis conditions (2 M NaOH and 16 h) resulted into maximum pCA release of 2.0 g/L. The pCA was separated from alkaline hydrolysate using sugaring out, a two phase separation method that results in aqueous phase and the organic solvent (acetonitrile) phase. Sugaring-out separated more than 90% of the pCA from the alkaline hydrolysate. Results of HPLC using standard pCA and FA showed that the main component of the separated top (organic solvent) phase was pCA rather than FA.