Abstract
The highly efficient and selective C(sp3)–S bond cross‐coupling method for the synthesis of 9‐thiolated fluorenes through a direct thiolation at 9‐C(sp3)–H of fluorenes with thiols is described. This reaction occurs at ambient conditions and shows good tolerance of functional groups including arylthiols and alkylthiols. A wide range of products is obtained in moderate to good yields. Besides, the reaction of benzothiophenol and fluorine generates unexpected 9‐benzylidene‐9H‐fluorene by eliminating hydrogen sulfide.
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