French-Iranian woman Rezai, 23, earned only her third career title after defeating fourth seed Williams 6-2, 7-5 in one hour and 41 minutes at La Caja Magica.
Rezai, who won in Bali and Strasbourg last year, swept aside Williams during a superb first set in which she broke her opponent in the third and seventh games before serving out to love to take the upper hand.
Serena suffers shock defeat It was a convincing start by Rezai, but she needed to dig deep during the second set to stage a remarkable fightback.
Williams, who had a 12-1 record on clay coming into the match, looked to be cruising towards levelling at one set all as she built a 5-2 lead and then, after Rezai had got back to 5-4, earning five set points on the Frenchwoman's serve in the 10th game.
However, Rezai saved all of them and, with the momentum behind her again, she broke Williams in the next game before serving out to win the match and the title.
Despite the loss Williams is set to return to second place in the world rankings for the first time since 2003 following her run this week, while she also won the women's doubles title at the Madrid Open with sister Serena last night.
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