Jacques Rudolph was unbeaten on 99 as Yorkshire closed 174 behind Surrey at 292-3 after two days at The Oval.
Mark Butcher completed his third double century and shared 232 with Australian Matt Nicholson, who made a career-best 133 as Surrey declared on 466-8.
Yorkshire had 20 minutes to bat before lunch and lost Joe Sayers for 14.
Anthony McGrath hit a rapid fifty with only 16 scoring shots before Rudolph, dropped on 75, hit 15 fours and shared an unbroken 162 with Andrew Gale (70).
Resuming on 189, Butcher recorded his 200 with a glorious cover drive.
He reached 205 when he was finally dismissed in the 102nd over, chipping to mid-wicket where Adil Rashid took a smart diving catch.
Nicholson played some strong shots on both sides of the wicket before he was bowled off his pads, and Butcher declared shortly afterwards.
West Indian Pedro Collins was soon in the wickets, a full-length delivery trapping Sayers and a yorker ending McGrath's enterprising innings.
Andrew Lyth played some pleasant shots before he was beaten by some sharp Saqlain Mushtaq turn and Butcher took a sharp catch high to his left at slip.
Saqlain should have added the scalps of both Rudolph and Gale, who were both missed in the slips, Gale when on just nine.
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