Good guesses so far, but no one has yet seized the cup. A reader calling himself Felix Frankfurter had the best guess so far with Hayburns Case. But Hayburns case provided details about the holdings of circuit courts striking down federal laws, while the Supreme Court in that case did not reach the question of judicial review or practice it in analyzing the statute, but rather merely recited what occurred below. Hayburns case is in fact the reason for my statement that I wanted a case in which the Supreme Court and not a circuit court exercised the power of judicial review. Good luck, and keep the guesses coming.
Ware v. Hylton, 3 U.S. (3 Dall.) 199 (1796).
In the case, the Supreme Court struck down a Virginia law (signed, I believe, by-then-governor Thomas Jefferson) that provided for the discharge of debts owed by Virginia citizens to subjects of Great Brittain. The court held that the state law contradicted the Tretay of Paris (1783) between the United States and Great Britain and was, therefore, invalid under the Supremacy clause.
Exparte Chandler and United States v. Yale Todd