Provided is a method for producing a radiohalogen-labeled compound, the method comprises: a step in which a radiohalogen-labeling precursor compound (S-L) having a leaving group (L) capable of being nucleophilically substituted by a radioactive halide ion (X−) is subjected to a radiohalogenation reaction to obtain a reaction mixture RM1 which contains the radiohalogen-labeling precursor compound (S-L) and a reaction product (S—X) resulting from the radiohalogenation reaction; a step in which the reaction mixture RM1 is mixed with a polyvalent acid or a salt thereof to obtain a reaction mixture RM2; and a step in which the reaction product (S—X) is purified from the reaction mixture RM2 by a solid phase extraction method.