One-pot synthesis of FePt nanoparticles larger than 5 nm with controlled composition has been developed by the polyol reduction of platinum acetylacetonate and iron acetylacetonate in excess ligands. The obtained large FePt nanoparticles (6.1 +/- 0.6 nm Fe36Pt64, 5.8 +/-0.7 nm Fe44Pt56, and 5.1 +/- 0.7 nm Fe49Pt51 nanoparticles) were thermally more stable than the small ones and were hard to coalesce in the in-plane direction for their 2D superlattice.