Extraction of copper and ammonia from Cu2+-NH3-Cl--H2O solution using laboratorialy synthesized sterically hindered β-diketone (4,4-dimethyl-1-(4-dodecylphenyl)-1,3-pentanedione) was studied. The effects of the copper concentration, the total ammonia concentration, the initial pH in the aqueous phase, the phase ratio, and the temperature on copper extraction ratio and ammonia extraction in loaded organic phase were investigated using this sterically hindered β-diketone. Under the conditions of temperature 25 °C, contact time of two phases 30 min, phase ratio 1:1, concentration of copper 3 g/L, concentration of total ammonia 3 mol/L, aqueous pH 8.43, and the concentration of β-diketone in organic phase 20% (volume fraction), ammonia in aqueous phase is much lower to be extracted by organic phase (just 14.5 mg/L), while the extraction rate of copper is 95.09%.