Semifluorinated n-alkanethiols, symmetrical sulfides and disulfides bearing the chain (s) F (CF2) n (CH2) m with n= 4, 6, 8, 10, and m= 2, 11 have been prepared by various synthetic methods, starting from the corresponding iodides or bromides. Methods based on sodium hydrogen sulfide, commonly used to accomplish this conversion, treatment of the Bunte salt obtained from sodium thiosulfate, the basic hydrolysis of isothiouronium salts, the ...