Weary Popyrin suffers agonising defeat in Cincinnati
Popyrin lost 7-6 (7-5) 6-7 (5-7) 5-7 after a see-saw encounter that could easily have gone the other way.
The Australian, himself ranked 19, will have the consolation of a very good workout ahead of the US Open, and may appreciate some rest after such a draining encounter. However, his chances of a top 16 ranking and better seeding slot in New York appear to be gone.
When Rublev's passing shot beat him to seal victory with the Russian's first match point Popyrin looked very weary, then smiled ruefully as he dragged himself to the net to give his opponent a hug.
The pair had slugged it out for three tight sets, interrupted in the last by a lengthy rain break.
First up on Court 3, in front of a decent crowd mainly supporting Rublev, Popyrin's opening serve was broken from 40-0 up, but he broke back immediately, helped by a brace of double-faults by the Russian.
The first set thereafter went with serve to the tiebreak. After four mini-breaks in that Popyrin served an ace at 5-5 then Rublev, facing set point, double-faulted.
The second set went with serve to the tiebreak, albeit Popyrin had to save three break points while forcing none. After double-faulting at 4-5 in the breaker he broke for 5-5, only for Rublev to sweep the next two points and the tiebreak.
The pair had been playing for more than two hours at this stage, in 32C heat. There followed an epic 28-point service game in which Popyrin forced but failed to take four break points.
The match had begun shortly after 11am local time, in fierce sunshine, but for some time humidity had been rising and clouds building. Suddenly, with the third set poised at 2-1 to Rublev, and 30-30 on Popyrin's serve, a cloudburst flooded the court and sent players and spectators rushing for cover.
Popyrin immediately went a break point down when they resumed just under an hour later, but saved it before serving out with two aces.
The match then went with serve until, at 30-30 and 5-6 down, the Australian had to step away from his serve due to a ringing mobile phone. It may have made no difference but his subsequent serves weren't quite there and Rublev pounced.
The Russian now meets Argentina's Francisco Comensana who beat Reilly Opelka 6-7 (4-7) 6-4 7-5.
Adam Walton is also in third round action, against Jiri Lehecka, the 22nd-seeded Czech. The winner will meet No.5 seed Ben Shelton or Roberto Bautista Agut in the last 16.
Elsewhere on Tuesday three-time grand slam semifinalist Grigor Dimitrov has withdrawn from the US Open, a little more than a month after he tore a chest muscle and had to quit playing against Jannik Sinner at Wimbledon.
Alejandro Tabilo gets his spot in the men's singles, which starts on August 24.
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