Abstract: The phase transfer catalyst Substituted Calix6arene was preparaed and it was used as catalyst to prepare the tumor diagnostic drug ¹⁸F-FET. The results showed that para-sulfonated-calix6arene not only catalyzes ¹⁹F substitution reaction, but also catalyzes ¹⁸F labelling reaction with radiochemical yield of 11%. However, para-tert-butyl-calix6arene has no catalytic activity for the ¹⁹F substitution reaction nor the ¹⁸F labelling reaction of the precursor of FET. The catalyzing of para-sulfonated-calix6arene may be related to it’s sulfonate groups, which participated in the coordination reaction and increased the polarity of calix6arene and so on. Although radiochemical yield of the para-sulfonated-calix6arene catalyzed ¹⁸F labeling of the precursor of FET was much lower than that obtained by Kryptofix 2.2.2, this study still has significant meaning for us to find better substituted Calix6arene catalysts by optimizing the reaction conditions.