May Days of Melies - Extraordinary Illusions [Dislocation mystérieuse] (1901)

The appropriately-named Extraordinary Illusions (aka Dislocation mystérieuse aka An Extraordinary Dislocation) features Méliès as a clown with the ability to detach his head and limbs, each of which develops a life of its own. This short also features the oldest existing appearance of a backdrop that Melies would use many more times, most famously in The Infernal Cakewalk.

http://www.imdb.com/title/tt0223146/