Gerard Moreno's penalty condemned Real Madrid to their second LaLiga defeat of the season as Villarreal beat the champions 2-1 on Saturday to do coach Quique Setien's former employers Barcelona a favour.
Madrid had hoped to return to the summit ahead of Barca's tough trip to Atletico Madrid on Sunday, but Villarreal were good value for victory during a thriller at Estadio de la Ceramica.
Villarreal created a host of promising openings during an entertaining first half but had to wait until just after the break to make the breakthrough thanks to Yeremy Pino.
Karim Benzema levelled with a spot-kick conceded by Juan Foyth on the hour mark, but the Argentinian then won one at the other end, with Moreno's confident finish ultimately sealing the win.
Villarreal had been the better side right from the start, going close after 28 seconds as Alex Baena sliced over. Francis Coquelin then saw an impudent backheeled finish clip the post following Alberto Moreno's low cross four minutes later.
Villarreal were indebted to Jose Reina just before the break, however, rushing out to deny Vinicius Junior.
The Yellow Submarine capitalised 65 seconds after the restart as Moreno released Yeremy into the box, his finish finding the net via deflections off Courtois and David Alaba.
Benzema spurned a glorious chance to level when Foyth blocked his goal-bound effort on the line, but the Frenchman made the most of his penalty reprieve after the defender's handball in the build-up was punished following a VAR review.
Villarreal went straight up the other end and won a penalty of their own moments later, though, Foyth seeing his pass handled by Alaba, and Moreno made no mistake.
Madrid's desperation led to Courtois going forward for a late corner and Arnaut Danjuma almost made it 3-1 on the break, though his inability to score into the empty goal did not matter.
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Villarreal fans were calling for Setien's dismissal just a few games into his reign earlier this season – they have now won six games in a row and are level on points with fourth-placed Atletico.
This was no mere fluke of a win either. Villarreal were genuinely much more inventive than Madrid, whose only real period of dominance came in the final 10 minutes as they pushed forward desperately.
There is every chance Diego Simeone and Atletico can conjure something against Barca on Sunday, so Madrid could yet end the weekend still level on points with the leaders, but Carlo Ancelotti will see this as an opportunity missed.
Villarreal's talisman the inspiration
There were several impressive performers for the hosts: Raul Albiol, Foyth and Dani Parejo were all exceptional, but Gerard Moreno was the star of the show.
He was at the heart of almost everything good about Villarreal's play, tallying a joint-high three key passes, including the assist for Yeremy, and he then held his nerve for the decisive penalty.
Vinicius and Foyth enjoy brilliant tussle
Vinicius was certainly lively here, but he found Foyth difficult to shake off as the Brazilian and Argentinian routinely duelled.
Foyth held his own in their battle, with his seven tackles at least four more than anyone else on the pitch.
Key Opta facts
– Villarreal have not lost their first LaLiga game of a calendar year since a 1-0 defeat to Real Madrid in 2009, winning eight (including the last four) and drawing six in this undefeated run.
– Following their loss to Getafe in 2022 (1-0), Madrid have now lost their first LaLiga game of a year in consecutive years for the first time since defeats in 1948 against CD Alcoyano (2-1) and in 1949 against Barcelona (3-1).
– Madrid have lost two of their last three away games in LaLiga (W1), just one fewer than in their previous 39 games on the road in the competition (W28 D8 L3).
– Madrid started a LaLiga game without a Spanish player in their ranks for the first time since Opta began collecting this data (21st century).
– Benzema has scored nine goals in 19 meetings with Villarreal in LaLiga, but only two of those have come away from home: in January 2019 (2-2) and in this game.
– Moreno has scored five goals in eight appearances for Villarreal against Madrid in LaLiga. This is more than any other Villarreal player has managed against Madrid in the competition. Here, he scored and assisted in a home league game for the first time since May 2021 against Sevilla.
Madrid head to Saudi Arabia for the Supercopa de Espana, which will pit them against Valencia in Wednesday's semi-final. Villarreal go to Celta Vigo two days later in LaLiga.