Both diastereoisomers of S-tert-butyl-β-(trifluoromethyl)isocysteine have been synthesized stereoselectivelyby the sequential reactions of trifluoroacetimidoyl chloridewith the lithium enolate of tert-butyl α-tert-butylthioacetate,followed by the diastereoselective reduction of the iminogroup with sodium borohydride in the presence of zinc(II)or di(ethylene glycol) dimethyl ether, and finally by thedeprotection of N-aryl and tert-butyl ester groups.